反応式
C[Si](N([Si](C)(C)C)C(=O)C(F)(F)F)(C)C.[NH2:16][C@@H:17]([CH2:21][C:22]#[N:23])[C:18]([OH:20])=[O:19].[CH2:24]([O:31][C:32](Cl)=[O:33])[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1>C(#N)C>[C:25]1([CH2:24][O:31][C:32]([NH:16][C@@H:17]([CH2:21][C:22]#[N:23])[C:18]([OH:20])=[O:19])=[O:33])[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1参加物
5
実験手順
Bis (trimethylsilyl)trifluoroacetamide (9.4 mL, 35 mmol.) was added to a suspension of (αS)-amino-3-cyanopropanoic acid (2.0 g., 17.5 mmol.) in 10 mL of dry acetonitrile and the reaction mixture was stirred for 3 hours. Benzylchloroformate (2.5 mL, 17.5 mmol) was added, the reaction mixture was stirred overnight, concentrated in vacuo, and dissolved in ethyl acetate (200 mL). The organic solution was washed with water (2×) and brine, dried (Na2SO4), and concentrated in vacuo. Crystallization from isopropyl ether yielded 3.82 g. of the title A product.
後処理
- stirringthe reaction mixture was stirred overnight
- concentrationconcentrated in vacuo
- dissolutiondissolved in ethyl acetate (200 mL)
- washThe organic solution was washed with water (2×) and brine
- dry with materialdried (Na2SO4)
- concentrationconcentrated in vacuo
- customCrystallization from isopropyl ether
- customyielded 3.82 g
出典と根拠
- ORDレコード
- ord-ee7f8a7636b943b6be7f4ce24c5ab941
- 出典データセット
- uspto-grants-1995_05
- 特許番号
- US05414017
関連ノート
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