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Pyridine → HCID 67362053, 화합물

HRID 2413540
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HRID 2413540 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(OCC)(OCC)O[CH2:28][CH3:29].C1(C)C=CC(S(O)(=O)=O)=CC=1.N1C=CC=CC=1>O1CCOCC1.CCOCC>[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][CH2:28][CH3:29])[CH2:18][CH2:19]1)=[CH:14][CH2:13]3)(=[O:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 1049PyridineHCID 6101p-Toluenesulfonic acidHCID 31214Ethyl orthoformateHCID 67361589Gestodene Impurity 1

생성물 1

HCID 67362053HCID 67362053, 화합물

시약·촉매·용매 2

HCID 3283Diethyl Ether용매
HCID 31275
1,4-Dioxane
용매

실험 절차

Under argon, 2.0 g of 15α-acetoxy-18-methyl-4-estrene-3,17-dione in 60 ml of dioxane is agitated at room temperature for 20 hours with 6 ml of triethyl orthoformate and 40 mg of p-toluenesulfonic acid. After adding 2 ml of pyridine, the mixture is diluted with ether, washed with water, and dried. The crude product is recrystallized from acetone/hexane. Yield: 1.6 g of 15α-acetoxy-3-ethoxy-18-methyl-3,5-estradien-17-one. Melting point: 202° C.

후처리

  1. washwashed with water
  2. customdried
  3. customThe crude product is recrystallized from acetone/hexane

출처 및 근거

ORD 기록
ord-b3aa82fe677d4f7ba0235dd4265c371f
출처 데이터셋
uspto-grants-1988_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04719054

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