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Triethylamine → 11beta-Fluoro-3-methoxyoestra-3,5-dien-17-one

HRID 900674
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HRID 900674 반응식
[F:1][C@H:2]1[CH2:19][C@@:17]2([CH3:18])[C@@H:13]([CH2:14][CH2:15][C:16]2=[O:20])[C@H:12]2[C@H:3]1[C@@H:4]1[C:9]([CH2:10][CH2:11]2)=[CH:8][C:7](=[O:21])[CH2:6][CH2:5]1.[NH+]1C=CC=C[CH:23]=1.C1(C)C=CC(S([O-])(=O)=O)=CC=1.C(N(CC)CC)C>COC(OC)(C)C.C(OCC)(=O)C>[F:1][C@H:2]1[CH2:19][C@@:17]2([CH3:18])[C@@H:13]([CH2:14][CH2:15][C:16]2=[O:20])[C@H:12]2[C@H:3]1[C@@H:4]1[C:9](=[CH:10][CH2:11]2)[CH:8]=[C:7]([O:21][CH3:23])[CH2:6][CH2:5]1
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참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 466102Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1)HCID 1097914511beta-Fluorooestr-4-ene-3,17-dione

생성물 1

HCID 1173826011beta-Fluoro-3-methoxyoestra-3,5-dien-17-one

시약·촉매·용매 2

HCID 64952,2-Dimethoxypropane용매
HCID 8857
Ethyl Acetate
용매

실험 절차

7.8 g of 11β-fluoro-estr-4-ene-3,17-dione (A′) was stirred in 40 ml of 2,2-dimethoxypropane with 780 mg of pyridinium-toluene-4-sulfonate for 5 hours at 80° C. Then, 1.5 ml of triethylamine was added. Then, it was diluted with ethyl acetate and washed with saturated sodium chloride solution. After crystallization from methanol, 5.3 g of 11β-fluoro-3-methoxy-estra-3,5-dien-17-one (A″) with a melting point of 173° C. was obtained.

후처리

  1. washwashed with saturated sodium chloride solution
  2. customAfter crystallization from methanol, 5.3 g of 11β-fluoro-3-methoxy-estra-3,5-dien-17-one (A″) with a melting point of 173° C.
  3. customwas obtained

출처 및 근거

ORD 기록
ord-c73adb54522f424bb8c643c351617319
출처 데이터셋
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07361645B2

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