HCID 15870673, 화합물 → HCID 86587645, 화합물

HRID 1837247노트

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HRID 1837247 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:4]1[CH:5]=[CH:6][C:7]([OH:27])=[CH:8][C:9]=1[CH2:10][C@H:11]2[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25]I.[F:28][C:29]([C:34]([F:40])([F:39])[C:35]([F:38])([F:37])[F:36])=[CH:30][CH2:31][NH:32][CH3:33]>CN1CCCC1=O>[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:4]1[CH:5]=[CH:6][C:7]([OH:27])=[CH:8][C:9]=1[CH2:10][C@H:11]2[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][N:32]([CH2:31][CH:30]=[C:29]([F:28])[C:34]([F:39])([F:40])[C:35]([F:36])([F:37])[F:38])[CH3:33]

참가 물질

4

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HCID 15870673HCID 15870673, 화합물HCID 54094144(3,4,4,5,5,5-Hexafluoro-pent-2-enyl)-methyl-amine

생성물 1

HCID 86587645HCID 86587645, 화합물수율 181.7%

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

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온도
80 °C

실험 절차

880 mg of 11β-fluoro-3-hydroxy-7α-(5-iodopentyl)-estra-1,3,5(10)-trien-17-one and 1.26 g of (3,4,4,5,5,5-hexafluoro-pent-2-enyl)-methyl-amine are dissolved in 20 ml of N-methylpyrrolidone and stirred for 3 hours at a bath temperature of 80° C. After the reaction solution is cooled to room temperature, the batch is added to saturated common salt solution, extracted with diethyl ether, dried and concentrated by evaporation in a vacuum. 1.86 g of 11β-fluoro-7α-{5-[(3,4,4,5,5,5-hexafluoro-pent-2-enyl)-methyl-amino]-pentyl}-3-hydroxy-estra-1,3,5(10)-trien-17-one is obtained as a crude product, which is used without purification in the next stage.

후처리

  1. temperatureAfter the reaction solution is cooled to room temperature
  2. additionthe batch is added to saturated common salt solution
  3. extractionextracted with diethyl ether
  4. customdried
  5. concentrationconcentrated by evaporation in a vacuum

출처 및 근거

ORD 기록
ord-fc2332eff411462090b54be13e0e4be2
출처 데이터셋
uspto-grants-2004_08
특허 번호
US06780855B2

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