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Ethyl orthoformate → HCID 67362053, 화합물

HRID 1472948
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HRID 1472948 반응식
C(OCC)(OCC)O[CH2:3][CH3:4].[C:11]([O:14][C@@H:15]1[C@H:21]2[C@H:22]3[C@H:31]([CH2:32][CH2:33][C@:18]2([CH2:19][CH3:20])[C:17](=[O:35])[CH2:16]1)[C@@H:30]1[C:25](=[CH:26][C:27](=[O:34])[CH2:28][CH2:29]1)[CH2:24][CH2:23]3)(=[O:13])[CH3:12]>CCO.C1(C)C=CC(S(O)(=O)=O)=CC=1>[C:11]([O:14][C@@H:15]1[C@H:21]2[C@H:22]3[C@H:31]([CH2:32][CH2:33][C@:18]2([CH2:19][CH3:20])[C:17](=[O:35])[CH2:16]1)[C@@H:30]1[C:25]([CH:26]=[C:27]([O:34][CH2:3][CH3:4])[CH2:28][CH2:29]1)=[CH:24][CH2:23]3)(=[O:13])[CH3:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 31214Ethyl orthoformateHCID 67361589Gestodene Impurity 1

생성물 1

HCID 67362053HCID 67362053, 화합물수율 97.2%

시약·촉매·용매 2

HCID 6101p-Toluenesulfonic acid촉매HCID 702Ethanol용매

실험 절차

Triethyl orthoformate (30 ml, 180 mmol) and p-Toluenesulfonic acid (300 mg, 1.57 mmol) were added to a suspension of 15α-acetoxy-18-methyl-estr-4-en-3,17-dione (30 g, 87 mmol) in EtOH (180 ml). The mixture was stirred at room temperature for 1 h, and then cooled to 0° C. The precipitate was filtered, washed with cooled ethanol and dried under vacuum to afford 15α-acetoxy-3-ethoxy-18-methyl-estra-3,5-dien-17-one (31.5 g, yield: 97%).

후처리

  1. temperaturecooled to 0° C
  2. filtrationThe precipitate was filtered
  3. washwashed with cooled ethanol
  4. customdried under vacuum

출처 및 근거

ORD 기록
ord-3ba8a172e94546c0a5e44fd874bb9193
출처 데이터셋
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09012667B2

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