Water → HCID 70505471, 화합물

HRID 2418143노트

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HRID 2418143 반응식
[OH:1][C@H:2]1[CH2:19][CH2:18][C@@:17]2([CH3:20])[C:4](=[CH:5][CH2:6][C@@H:7]3[C@@H:16]2[CH2:15][CH2:14][C@@:12]2([CH3:13])[C@H:8]3[C@@H:9]3[CH2:22][C@@H:10]3[C:11]2=[O:21])[CH2:3]1.[C:23](Cl)(=[O:30])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.O>N1C=CC=CC=1.C(Cl)Cl>[C:23]([O:1][C@H:2]1[CH2:19][CH2:18][C@@:17]2([CH3:20])[C:4](=[CH:5][CH2:6][C@@H:7]3[C@@H:16]2[CH2:15][CH2:14][C@@:12]2([CH3:13])[C@H:8]3[C@@H:9]3[CH2:22][C@@H:10]3[C:11]2=[O:21])[CH2:3]1)(=[O:30])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1

참가 물질

6

반응물 3

HCID 962WaterHCID 7412Benzoyl chlorideHCID 1307594915,16-Dihydro-3-hydroxy-3'H-cycloprop[15,16]androsta-5,15-dien-17-one

생성물 1

HCID 70505471HCID 70505471, 화합물

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 6344Dichloromethane용매

실험 절차

A solution of 5.0 g of 3β-hydroxy-15β,16β-methylene-5-androsten-17-one in 50 ml of pyridine was combined under ice cooling with 5 ml of benzoyl chloride and then stirred for 17 hours at room temperature. After the addition of 10 ml of water, the mixture was stirred for another hour; then the reaction solution was diluted with methylene chloride and washed with sodium carbonate solution and water. After drying and evaporation, the residue was triturated with diisopropyl ether and vacuum-filtered, thus obtaining 6.4 g of 3β-benzoyloxy-15β,16β-methylene-5-androsten-17-one, mp 250°-258° C.

후처리

  1. stirringthe mixture was stirred for another hour
  2. washwashed with sodium carbonate solution and water
  3. customAfter drying
  4. customevaporation
  5. customthe residue was triturated with diisopropyl ether
  6. filtrationvacuum-filtered

출처 및 근거

ORD 기록
ord-420ed9d9aef647808eb71a6a51a8fca1
출처 데이터셋
uspto-grants-1984_09
특허 번호
US04472310

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