反応 #947

反応方程式

Chlorosulphonic acid

product

(+-)-2-Amino-2-ethylhex-4-en-1-ol

→

desired product

収率 57.0%

(+-)-2-But-2-enyl-2-ethylaziridine

収率 57.0%

溶媒

acetonitrile

反応条件

後処理

1. 1
   workup.ADDITIONWhen addition
2. 2
   ろ過The resulting crystals were filtered off
3. 3
   洗浄washed with acetonitrile/pet. ether
4. 4
   その他dried
5. 5
   workup.ADDITIONtaken up in a mixture of 50%
6. 6
   workup.DISTILLATIONKOH (100 mL) and water (55 mL) and distilled over KOH

実験手順

Chlorosulphonic acid (18 mL) was added to a solution of the product from step (e) (32.3 g) in acetonitrile (100 ml) at least 9° C. When addition was complete, the mixture was warmed to room temperature. The resulting crystals were filtered off, washed with acetonitrile/pet. ether, dried, taken up in a mixture of 50% w/v aqu. KOH (100 mL) and water (55 mL) and distilled over KOH to give the desired product as a colourless oil (16.1 g). 1H NMR consistent with the proposed structure.

出典