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

HRID 1472955
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HRID 1472955 반응식
[C:1]1(C)C=CC(S([O-])(=O)=O)=CC=1.[NH+]1C=CC=CC=1.[C:18]([O:21][C@@H:22]1[C@H:28]2[C@H:29]3[C@H:38]([CH2:39][CH2:40][C@:25]2([CH2:26][CH3:27])[C:24](=[O:42])[CH2:23]1)[C@@H:37]1[C:32](=[CH:33][C:34](=[O:41])[CH2:35][CH2:36]1)[CH2:31][CH2:30]3)(=[O:20])[CH3:19]>COC(OC)(C)C>[C:18]([O:21][C@@H:22]1[C@H:28]2[C@H:29]3[C@H:38]([CH2:39][CH2:40][C@:25]2([CH2:26][CH3:27])[C:24](=[O:42])[CH2:23]1)[C@@H:37]1[C:32]([CH:33]=[C:34]([O:41][CH3:1])[CH2:35][CH2:36]1)=[CH:31][CH2:30]3)(=[O:20])[CH3:19]
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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 498.3%

시약·촉매·용매 1

HCID 64952,2-Dimethoxypropane용매

실험 절차

Pyridinium p-Toluenesulfonate (260 mg, 1.03 mmol) was added to a suspension of 15α-acetoxy-18-methyl-estr-4-en-3,17-dione (2 g, 5.8 mmol) in 2,2-dimethoxypropane (20 ml). The mixture was stirred under reflux for 7 h and at room temperature overnight. It was then cooled to −10° C. for 1 h. The precipitate was filtered, washed with cooled MeOH and dried under vacuum to afford 15α-acetoxy-3-methoxy-18-methyl-estra-3,5-dien-17-one (1.84 g, yield: 88%).

후처리

  1. temperatureIt was then cooled to −10° C. for 1 h
  2. filtrationThe precipitate was filtered
  3. washwashed with cooled MeOH
  4. customdried under vacuum

출처 및 근거

ORD 기록
ord-5b3c7ecdd6b34e39a35327d40c3fa461
출처 데이터셋
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09012667B2

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