Pyridine → 3-(Chloromethoxycarbonyl) Cholesterol

HRID 1406

反応式

HRID 1406 の反応式
Cl[C:2]([O:4][CH2:5][Cl:6])=[O:3].[CH3:7][CH:8]([CH2:10][CH2:11][CH2:12][C@H:13]([C@@H:15]1[C@:33]2([CH3:34])[C@H:18]([C@H:19]3[C@H:30]([CH2:31][CH2:32]2)[C@:28]2([CH3:29])[C:22]([CH2:23][C@H:24]([CH2:26][CH2:27]2)[OH:25])=[CH:21][CH2:20]3)[CH2:17][CH2:16]1)[CH3:14])[CH3:9].N1C=CC=CC=1>C(Cl)Cl>[Cl:6][CH2:5][O:4][C:2]([C@:24]1([OH:25])[CH2:26][CH2:27][C@@:28]2([CH3:29])[C:22](=[CH:21][CH2:20][C@@H:19]3[C@@H:30]2[CH2:31][CH2:32][C@@:33]2([CH3:34])[C@H:18]3[CH2:17][CH2:16][C@@H:15]2[C@H:13]([CH3:14])[CH2:12][CH2:11][CH2:10][CH:8]([CH3:9])[CH3:7])[CH2:23]1)=[O:3]

参加物

5

反応物 3

HCID 1049PyridineHCID 5997CholesterolHCID 62754Chloromethyl chloroformate

生成物 1

HCID 571798753-(Chloromethoxycarbonyl) Cholesterol

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

Chloromethyl chloroformate (1.96 g, 15.2 mmol) and cholesterol (5.0 g, 12.9 mmol) was dissolved in CH2Cl2 (10 ml). The solution was cooled. Pyridine (1.21 g, 15.3 mmol) was dripped into the stirred solution over 5 minutes. Heat was produced and the reaction gave a clear solution from a somewhat unclear starting solution. After 24 hours at room temperature, the mixture was diluted with CH2Cl2 (50 ml), washed with 0.5M HCl (50 ml) and water (3×25 ml). After treatment with MgSO4, the solution was evaporated to dryness.

後処理

  1. temperatureThe solution was cooled
  2. temperatureHeat
  3. customwas produced
  4. customthe reaction gave a clear solution from
  5. washwashed with 0.5M HCl (50 ml) and water (3×25 ml)
  6. customAfter treatment with MgSO4, the solution was evaporated to dryness

出典と根拠

ORDレコード
ord-169f88b27a294c15b3d94e8de0e682c6
出典データセット
uspto-grants-1998_03
特許番号
US05725840

関連ノート

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