反応式
[C:1]([NH:11][C@H:12]([C:17]([OH:19])=[O:18])[CH2:13][C:14]([OH:16])=O)([O:3][CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)=[O:2]>C(OC(=O)C)(=O)C>[CH2:4]([O:3][C:1]([NH:11][C@@H:12]1[C:17](=[O:18])[O:19][C:14](=[O:16])[CH2:13]1)=[O:2])[C:5]1[CH:6]=[CH:7][CH:8]=[CH:9][CH:10]=1参加物
3
反応条件
- 温度
- 75 °C
実験手順
The above illustrated starting compound which is commercially available N-CBZ aspartic acid (205.7 g, 0.77 mol) was added to acetic anhydride (300 ml). This mixture was stirred at 75° C. for 4 hours. The excess acetic anhydride and acetic acid byproduct were distilled from the mixture under reduced pressure and the residue was recrystallised from hot dichloromethane. The product was collected by filtration, washed with hexane and dried at ambient temperature under reduced pressure to give a white fluffy solid.
後処理
- distillationThe excess acetic anhydride and acetic acid byproduct were distilled from the mixture under reduced pressure
- customthe residue was recrystallised from hot dichloromethane
- filtrationThe product was collected by filtration
- washwashed with hexane
- customdried at ambient temperature under reduced pressure
- customto give a white fluffy solid
出典と根拠
- ORDレコード
- ord-f220232a1ce74980bd2c13304127a203
- 出典データセット
- uspto-grants-1998_11
- 特許番号
- US05840667
関連ノート
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