How is a clothes dryer a sieve
1. Synthesis of Diethyl Benzyloxy-Methyl-Malonate (Ergovaline)
all right well I'm going to try to weigh
out three point nine six five grams of
60% sodium hydride this stuff that's
eaten away at the plastic bag that was
originally in quite a bit but I think
it's still good
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I can try not to get plastic pieces in
here
right close them I did heat this with a
heat gun so it should be relatively dry
but I am going to open it to throw this
in here three point nine nine three
grams and this one I'm running two of
them so it's going to do it again the
only reason I'm running to is click
don't have a two liter flask and I only
have one liter left this way if I screw
up on one least I have the other ones in
it but I am making it double to work all
right should be in there close enough to
three point nine six five there is a
little bit of those yellow plastic
pieces
hopefully won't matter too much just to
make sure the sodium hydride is still
good and some water here I have a little
bit of it still stuck on this so still
good should react looks pretty good to
me right now I'm just going to add 250
no leader of toluene through each of
these left
I will now add about ten point three
milliliters of benzyl alcohol
I do see some bubbles so maybe
something's happening but it's hard to
tell it's just kind of stirring or
reacting all right looks like it's all
added I'll do the same thing for this
flash this one certainly looks like it's
reacting more this one bubbling up quite
a bit how do you even see it so white
Wow I wonder why this one foaming so
much and the other one did all right
that one's done as well now to this one
mole equivalent of the benzyl alcohol
are approximately 1 mol equivalent
relative to the sodium hydride there
this one's still going good this one
doesn't look like it's foaming at all
this one all sorts of puzzles all right
so now I'm going to hook up condensers
to each of them so I can reflux them for
an hour make sure it does go to
completion
Wow yes yes
all right just turn down the water so
the condenser looks like that's working
out okay the layers are set up I just
have drying shoot at the top of the
condensers I did take a heat gun ahead
of time and I did try to get rid of the
water as much as I could from the
condensers and the drying tube now I'll
just get it to reflux all right so it's
only it's been about 10 minutes maybe 15
at the most this oil baths up to 81 this
one's at 68 both of these solutions are
looking a little funny for its color
they both look tan or brown light brown
I don't know I guess can - better
stripped it for it
this shouldn't be because the salt
itself is white and I'm guessing it's
this color just because of those little
plastic pieces which were discolored
actually but I mean there's little
chunks in there that
that looks like they're red or black I'm
I'm hoping that's what's influencing the
color here and it's just a small amount
color doesn't necessarily mean a whole
lot so hopefully everything will still
work out all right so it's only been a
few more minutes maybe 25 minutes total
and this one is boiling already it's at
99 degrees Celsius
you see it's becoming very gel-like and
can't even see it really stirring
anymore
looks like the condensers working fine
only have some condensate up this far
nothing higher than that another
solution is at 84 degrees Celsius not
quite boiling yet not quite solidified
yet if you have some stuff that looks
like it got up here though
the condenser too as well working just
fine it looks like the condensate the
farthest got to the bunch of this line
been about an hour since they both
started to reflux
he's only this one started a little bit
earlier I'm going to go ahead and stop
them both this one did start spinning
again and it looks like it's a little
bit less viscous now this one is really
spinning well hopefully everything's
okay still seems like there's a lot of
salt there it's just not as
biscuit as I thought it would be
this one certainly has a lot more it
would seem but anyway stop them both let
them cool down to room temperature I'll
throw them in some ice
all right they both should be cooled now
in the ice water bath
and now I'm going to add on 18.9 Mills
are 25 grams of the diethyl bromo methyl
melanie can't really see anything
happening
if it was a big solid clump it should
start dissolving as this is added but
since it's already stirring well can't
really tell although it does seem to be
doing better and better as I add this
fill most becoming transparent
looking pretty good at that I can almost
see the stir bar again alright that's
the last of it look at that
not bad remember it looked like this so
I'll go ahead and least take this out of
the ice water bath for now completely
transparent now no salt at all left
anymore which is a pretty good sign as
you can do the same thing with this one
this one still has some salt up here but
I will keep this
all right there we go the condensers are
hooked back up and now I'm just going to
heat it to about 70 degrees Celsius for
four hours
all right been four hours since the
temperature has been between somewhere
between 60 and looks like the highest
now it's been at this one seventy one
point six this one is at six to nine
point seven that's probably as high as
temperature too but anyway between 60
degrees and 72 degrees Celsius for at
least four hours mostly around 65 I'm
going to go ahead and quench this with
20 mils of water look at all that salt
there
all right so go ahead and transfer it
over to the secretory cell oh I dropped
the stir bar in there
have a little toluene here and skin
rinse this out once anyway so I'll be
able to wash back whatever little amount
for that hat stir bar
there's certainly two layers there I
thought about adding some more water to
dissolve this but I don't think I need
to I think it's just going to come out
with the water layer for the most part
I still had more water this time I got
measured at 35 milliliters
then I will collect let's call you mean
that should have my product in it as
well
now hopefully it'll clear itself up to
get rid of that water
doesn't look like it's going to do the
trick
sorry I'm Kennedy Kansas in 2000 middle
flat
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still kind of a free-flowing liquid in
there alright so I'm going to drive
again
doesn't look like it's very wet because
the sodium sulfate did not come up at
all so that's a good sign
it is so cloudy though probably because
the toluene I guess that's okay I need
to transfer it to another flask anyway
when I would just use dichloromethane
this time
looking pretty clear now
all right so here they both are should
be completely wrote a bath down they
both don't smell like any solvents they
smell sweet like a obn should this one I
have 27 point one seven one gram and the
other one twenty seven point nine three
four grams so the proton is done
there it is
here's a triplet for the two ch3 groups
off the ethyl ester here's the
corresponding quartet for the two ch2
groups here is the singlet or the methyl
group here's the singlet for the ch2
from the spindle oxy and here are the
five aromatic hydrogen
