반응 #1274

반응 방정식

acetonitrile

Methanesulfonic acid

Indene oxide

Water

→

cis 1-amino-2-indanol

용매

methylene chloride

반응 조건

후처리

1. 1
   온도The mixture was warmed to 25° C. and aged for 2 h
2. 2
   온도the mixture heated at 45° C. for 5 h
3. 3
   기타The organic phase was separated
4. 4
   온도the aqueous phase further heated
5. 5
   온도at reflux for 4 h with concentration to approximately 200 g/L
6. 6
   온도cooled to 5° C.
7. 7
   여과filtered
8. 8
   기타dried in vacuo

실험 절차

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.

출처