Acetone → Ethyl phenylglycinate, D-
反応式
[CH3:1][CH2:2][O:3][C:4]([CH:6]([NH2:13])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)=[O:5].C(O)(=O)C(C(C(O)=O)O)O.CC(C)=O>C(O)C>[CH3:1][CH2:2][O:3][C:4]([C@H:6]([NH2:13])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)=[O:5]参加物
5
実験手順
A solution of ethyl DL-phenylglycinate (5.00 g., 28 mmole) and (+)-tartaric acid (4.18 g., 28 mmole, 1 equiv.) in ethanol (50 ml.) was made at 58°. The solution was cooled, acetone (4.1 ml., 55.6 mmole, 2 equiv.) was added and the mixture was stirred at 20° to 25° for 165 hours. The solid was filtered off, washed with ethanol (2 × 10 ml.) and dried at 26°/2 mm. for 41/2 hours to give ethyl D-phenylglycinate (+)-hemitartrate as a monoethanol solvate (9.338 g., 89%), [α]D -46.5° (c 2.5 H2O).
後処理
- customwas made at 58°
- temperatureThe solution was cooled
- filtrationThe solid was filtered off
- washwashed with ethanol (2 × 10 ml.)
- customdried at 26°/2 mm
出典と根拠
- ORDレコード
- ord-81da3982a726476eadb90ec3b57d2021
- 出典データセット
- uspto-grants-1976_08
- 特許番号
- US03976680
反応ノート
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