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Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) → HCID 67362263, 화합물

HRID 1472969
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HRID 1472969 반응식
[C:1]([O:4][C@@H:5]1[C@H:11]2[C@H:12]3[C@H:21]([CH2:22][CH2:23][C@:8]2([CH2:9][CH3:10])[C:7](=[O:25])[CH2:6]1)[C@@H:20]1[C:15](=[CH:16][C:17](=[O:24])[CH2:18][CH2:19]1)[CH2:14][CH2:13]3)(=[O:3])[CH3:2].[C:26]1(C)C=CC(S([O-])(=O)=O)=CC=1.[NH+]1C=CC=CC=1>COC(OC)(C)C>[C:1]([O:4][C@@H:5]1[C@H:11]2[C@H:12]3[C@H:21]([CH2:22][CH2:23][C@:8]2([CH2:9][CH3:10])[C:7](=[O:25])[CH2:6]1)[C@@H:20]1[C:15]([CH:16]=[C:17]([O:24][CH3:26])[CH2:18][CH2:19]1)=[CH:14][CH2:13]3)(=[O:3])[CH3:2]
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참가 물질

4

반응물 2

HCID 466102Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1)HCID 67361589Gestodene Impurity 1

생성물 1

HCID 67362263HCID 67362263, 화합물수율 623.6%

시약·촉매·용매 1

HCID 64952,2-Dimethoxypropane용매

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온도
-10 °C

실험 절차

A suspension of 15α-acetoxy-18-methyl-estr-4-en-3,17-dione (48 g, 139 mmol) and pyridinium p-Toluenesulfonate (4.8 g, 19.1 mmol) in 2,2-dimethoxypropane (400 ml) was refluxed for 6 h. The mixture was then cooled to −10° C. for 2 h. The precipitate was filtered, washed with cooled methanol and dried under vacuum to afford 15α-acetoxy-3-methoxy-18-methyl-estra-3,5-dien-17-one (42.7 g, yield: 86%).

후처리

  1. temperaturewas refluxed for 6 h
  2. filtrationThe precipitate was filtered
  3. washwashed with cooled methanol
  4. customdried under vacuum

출처 및 근거

ORD 기록
ord-bb05dcf7331e48d9bcebf28bd68a215c
출처 데이터셋
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09012667B2

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