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Hydrochloric Acid → Benzyl ((2R,3S)-4-chloro-3-hydroxy-1-(phenylthio)butan-2-yl)carbamate

HRID 2304789
ノート
印刷プレビュー

反応式

HRID 2304789 の反応式
CC(C)[O-].[Al+3].CC(C)[O-].CC(C)[O-].[Cl:14][CH2:15][C:16](=[O:37])[C@@H:17]([NH:26][C:27](=[O:36])[O:28][CH2:29][C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1)[CH2:18][S:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1.Cl>C(O)(C)C>[Cl:14][CH2:15][C@@H:16]([OH:37])[C@@H:17]([NH:26][C:27](=[O:36])[O:28][CH2:29][C:30]1[CH:31]=[CH:32][CH:33]=[CH:34][CH:35]=1)[CH2:18][S:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 11143Aluminum isopropoxideHCID 10808734(R)-Benzyl (4-chloro-3-oxo-1-(phenylthio)butan-2-yl)carbamate

生成物 1

HCID 9951031Benzyl ((2R,3S)-4-chloro-3-hydroxy-1-(phenylthio)butan-2-yl)carbamate収率 80%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

反応条件

温度
50 °C

実験手順

To a suspension of 2.15 g aluminium isopropoxide in 35 ml of isopropanol were added 3.64 g of benzyl [3-chloro-2-oxo-(R)-1-(phenylthiomethyl)-propyl]-carbamate and the mixture was stirred at 50° C./400mbar for 4 hours. The mixture was cooled to 0° C., the pH was adjusted to 1 by adding hydrochloric acid and the isopropanol was evaporated. The residue was partitioned between water and dichloromethane and the organic layer was evaporated. The residue was chromatographed on silica to give 2.9 g (80%) of pure benzyl (1R, 2S)-[3-chloro-2-hydroxy-1-(phenylthiomethyl)-propyl]-carbamate. IR (KBr): 3360 br (NH, OH), 1690 s (C═O), 1540 s (amide II).

後処理

  1. temperatureThe mixture was cooled to 0° C.
  2. customthe isopropanol was evaporated
  3. customThe residue was partitioned between water and dichloromethane
  4. customthe organic layer was evaporated
  5. customThe residue was chromatographed on silica

出典と根拠

ORDレコード
ord-106029996b244de398fb9a9adfe762ed
出典データセット
uspto-grants-2002_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06437134B1

反応ノート

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