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Water → HCID 67362260, 화합물

HRID 1472958
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HRID 1472958 반응식
C(N(CC)CC)C.C(O[C@@H:12]1[C@H:18]2[C@H:19]3[C@H:28]([CH2:29][CH2:30][C@:15]2([CH2:16][CH3:17])[C:14](=[O:32])[CH2:13]1)[C@@H:27]1[C:22](=[CH:23][C:24](=[O:31])[CH2:25][CH2:26]1)[CH2:21][CH2:20]3)(=O)C.O>CCO>[CH3:17][CH2:16][C@:15]12[CH2:30][CH2:29][C@H:28]3[C@@H:19]([CH2:20][CH2:21][C:22]4[C@@H:27]3[CH2:26][CH2:25][C:24](=[O:31])[CH:23]=4)[C@@H:18]1[CH:12]=[CH:13][C:14]2=[O:32]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 8471TriethylamineHCID 67361589Gestodene Impurity 1

생성물 1

HCID 67362260HCID 67362260, 화합물수율 62%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Triethylamine (4 ml, 28.7 mmol) was added to a suspension of 15α-acetoxy-18-methyl-estr-4-en-3,17-dione (4 g, 11.6 mmol) in EtOH (24 ml). The mixture was heated under reflux for 2 h. It was cooled to room temperature and water (50 ml) was added. The precipitate was filtered, washed with a 6/4 EtOH/water solution and dried under vacuum. The residue was purified by flash chromatography on silica gel to afford 18-methyl-estra-4,15-dien-3,17-dione (2 g, yield: 62%).

후처리

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 2 h
  3. filtrationThe precipitate was filtered
  4. washwashed with a 6/4 EtOH/water solution
  5. customdried under vacuum
  6. customThe residue was purified by flash chromatography on silica gel

출처 및 근거

ORD 기록
ord-0bd93415cadc4004bf89607adc57d30e
출처 데이터셋
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09012667B2

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