反応 #1274

反応方程式

acetonitrile

Methanesulfonic acid

Indene oxide

Water

→

cis 1-amino-2-indanol

溶媒

methylene chloride

反応条件

後処理

1. 1
   温度The mixture was warmed to 25° C. and aged for 2 h
2. 2
   温度the mixture heated at 45° C. for 5 h
3. 3
   その他The organic phase was separated
4. 4
   温度the aqueous phase further heated
5. 5
   温度at reflux for 4 h with concentration to approximately 200 g/L
6. 6
   温度cooled to 5° C.
7. 7
   ろ過filtered
8. 8
   その他dried in vacuo

実験手順

Indene oxide (117 g) diluted to a total volume of 600 mL in methylene chloride was diluted with acetonitrile (600 mL) and cooled to -20° C. Methanesulfonic acid (114 mL) was then added. The mixture was warmed to 25° C. and aged for 2 h. Water (600 mL) was added and the mixture heated at 45° C. for 5 h. The organic phase was separated and the aqueous phase further heated at reflux for 4 h with concentration to approximately 200 g/L. The solution was adjusted to pH 12.5 with 50% aqueous sodium hydroxide, and then cooled to 5° C. and filtered, dried in vacuo, to provide cis 1-amino-2-indanol.

出典