Water → (1R,2S)-(+)-cis-1-Amino-2-indanol
反応式
[CH:1]12[O:10][CH:2]1[CH2:3][C:4]1[C:9]2=[CH:8][CH:7]=[CH:6][CH:5]=1.CS(O)(=O)=O.O.C(#[N:19])C>C(Cl)Cl>[NH2:19][C@@H:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH2:3][C@@H:2]1[OH:10]参加物
6
反応条件
- 温度
- -20 °C
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.
後処理
- temperatureThe mixture was warmed to 25° C. and aged for 2 h
- temperaturethe mixture heated at 45° C. for 5 h
- customThe organic phase was separated
- temperaturethe aqueous phase further heated
- temperatureat reflux for 4 h with concentration to approximately 200 g/L
- temperaturecooled to 5° C.
- filtrationfiltered
- customdried in vacuo
出典と根拠
- ORDレコード
- ord-5cabef20e3d4416cbf3328a8863028c7
- 出典データセット
- uspto-grants-1998_03
- 特許番号
- US05723615
反応ノート
読み込み中…