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Methanesulfonyl chloride → HCID 86736736, 화합물

HRID 1448020
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HRID 1448020 반응식
[OH:1][C@@H:2]1[CH2:27][CH2:26][C@@:25]2([CH3:28])[C@H:4]([C@@H:5]([OH:30])[CH2:6][C@@H:7]3[C@@H:24]2[CH2:23][CH2:22][C@@:21]2([CH3:29])[C@H:8]3[CH2:9][CH2:10][C@@H:11]2[C@H:12]([CH3:20])[CH2:13][CH2:14][C:15](=[O:19])[CH:16]([CH3:18])[CH3:17])[CH2:3]1.[CH3:31][S:32](Cl)(=[O:34])=[O:33]>N1C=CC=CC=1>[S:32]([OH:34])(=[O:1])(=[O:33])[CH3:31].[S:32]([OH:34])(=[O:1])(=[O:33])[CH3:31].[OH:1][C@@H:2]1[CH2:27][CH2:26][C@@:25]2([CH3:28])[C@H:4]([C@@H:5]([OH:30])[CH2:6][C@@H:7]3[C@@H:24]2[CH2:23][CH2:22][C@@:21]2([CH3:29])[C@H:8]3[CH2:9][CH2:10][C@@H:11]2[C@H:12]([CH3:20])[CH2:13][CH2:14][C:15](=[O:19])[CH:16]([CH3:18])[CH3:17])[CH2:3]1
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참가 물질

4

반응물 2

HCID 31297Methanesulfonyl chlorideHCID 22809505HCID 22809505, 화합물

생성물 1

HCID 86736736HCID 86736736, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

To the solution of 3α,6α-dihydroxy-5β-cholestan-24-one (168 mg) in pyridine (5 ml) was added methanesulfonyl chloride (0.5 ml) under cooling in an ice bath and the mixture was continuously stirred for one hour. The reaction mixture was poured into ice-water and extracted with ethyl acetate. The ethyl acetate layer was washed with an aqueous solution of hydrochloric acid and then with water, dried over magnesium sulfate and evaporated to give an oily product, 3α,6α-dihydroxy-5β-cholestan-24-one dimesylate.

후처리

  1. temperatureunder cooling in an ice bath
  2. extractionextracted with ethyl acetate
  3. washThe ethyl acetate layer was washed with an aqueous solution of hydrochloric acid
  4. dry with materialwith water, dried over magnesium sulfate
  5. customevaporated

출처 및 근거

ORD 기록
ord-dba2060148904e29b858a42108334d8f
출처 데이터셋
uspto-grants-1979_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04179452

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