Water → HCID 10673665, 화합물

HRID 233508노트

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HRID 233508 반응식
[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

참가 물질

6

반응물 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 31297Methanesulfonyl chlorideHCID 10503609HCID 10503609, 화합물

생성물 1

HCID 10673665HCID 10673665, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매2회

반응 조건

온도
-25 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-7605d7b20a6c402d803718d3be41ffed
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05593983

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