Chemistry Reference
In-Depth Information
Planetary Ball Mill
CO 2
R 1
1) Activating Agent 37 / DMAP
R 1
Waste
water soluble salts
300-450 rpm (Cycled milling )
OH
OR 3
+
R 2 HN
R 2 HN
OH
10 min x 6 / 50 balls
( t- BuOH)
(in the case
of Boc 2 O)
O
O
2) Aqueous acidic work-up
N
O
O
36
R 2 = CO 2 t Bu, COCH 2 Ph
38
18 examples
35-91%
(in the case
of DSC)
O
R 3 O
Y
2) Aqueous acidic work-up
37
DMAP
N
R 1
DMAP
R 1
R 2
O
OR 3
(cat.)
R 2
N
H
O
H
R 3 = Me, Et, CHCH 2 =CH 2 ,
CH 2 Ph (ZCl)
O
O
O
R 3 O
Cl
OR 3
OR 3
CO 2
A
B
O
Mixed carboxylic-carbonic
anhydride
O
O
O
R 3 =
R 3
R 3
N
(DSC),
Me (DMC)
=
O
R 3 O
Y
O
37
R 3 O
OR 3
O
R 3 =
t- Bu (Boc 2 O)
CH 2 Ph (Z 2 O)
Me (Moc 2 O)
Activating agent
O
O
Scheme 6.10 C-Terminal esterification for protection/activation of N-protected amino acids in a planetary ball-mill.
 
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