Water → HCID 10673665、化合物

HRID 233508ノート

反応式

HRID 233508 の反応式
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[OH:6][C@@H:7]1[C@@H:27]([N:28]2[CH2:33][CH2:32][O:31][C:30]([CH3:35])([CH3:34])[CH2:29]2)[CH2:26][C@@:25]2([CH3:36])[C@@H:9]([CH2:10][CH2:11][C@@H:12]3[C@@H:24]2[CH2:23][CH2:22][C@@:21]2([CH3:37])[C@H:13]3[CH2:14][CH2:15][C@@H:16]2[C:17](=[O:20])[CH2:18][OH:19])[CH2:8]1.O.C(=O)([O-])[O-].[Na+].[Na+]>N1C=CC=CC=1>[OH:6][C@@H:7]1[C@@H:27]([N:28]2[CH2:33][CH2:32][O:31][C:30]([CH3:35])([CH3:34])[CH2:29]2)[CH2:26][C@@:25]2([CH3:36])[C@@H:9]([CH2:10][CH2:11][C@@H:12]3[C@@H:24]2[CH2:23][CH2:22][C@@:21]2([CH3:37])[C@H:13]3[CH2:14][CH2:15][C@@H:16]2[C:17](=[O:20])[CH2:18][O:19][S:2]([CH3:1])(=[O:4])=[O:3])[CH2:8]1

参加物

6

反応物 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 31297Methanesulfonyl chlorideHCID 10503609HCID 10503609、化合物

生成物 1

HCID 10673665HCID 10673665、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒2 回

反応条件

温度
-25 °C

実験手順

A solution of methanesulfonyl chloride (2.48 ml) in dry pyridine (9.6 ml) was added to a solution of the 3,21-dihydroxy compound of Example 9 (3.26 g) in dry pyridine (33 ml) at -25° C. over ca. 5 min. The solution was stirred at -25° C. for 1.5 h and poured into water (400 ml). Aqueous sodium carbonate was added until the pH exceeded 9 and the precipitated solid was filtered off and dissolved in dichloromethane. The solution was dried over sodium sulfate and the solvent was removed under reduced pressure to give (2β,3α,5α)-3-hydroxy-2-(2,2-dimethyl-4-morpholinyl)-21-[(methylsulfonyl)oxy]pregnan-20-one (3.80 g). δ (CDCl3) 0.65 (s,3H), 0.86 (s,3H), 3.22 (s,3H) and 4.79 (m,2H).

後処理

  1. filtrationthe precipitated solid was filtered off
  2. dissolutiondissolved in dichloromethane
  3. dry with materialThe solution was dried over sodium sulfate
  4. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-7605d7b20a6c402d803718d3be41ffed
出典データセット
uspto-grants-1997_01
特許番号
US05593983

反応ノート

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