Sodium Chloride → HCID 86587645, 화합물

HRID 1838914노트

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HRID 1838914 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].[Cl-].[Na+]>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

5

반응물 3

HCID 5234Sodium ChlorideHCID 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)oestra-1,3,5(10)-trien-17-one and 1.26 g of (3,4,4,5,5,5-hexa-fluoropent-2-enyl)methylamine are dissolved in 20 ml of N-methylpyrrolidone and stirred at a bath temperature of 80° C. for 3 hours. After the reaction solution has cooled to room temperature, the mixture is added to saturated sodium chloride solution, extracted with diethyl ether, dried and concentrated in vacuo. 1.86 g of 11β-fluoro-7α-{5-[(3,4,4,5,5,5-hexafluoropent-2-enyl)methylamino]pentyl}-3-hydroxyestra-1,3,5(10)-trien-17-one are obtained as a crude product which is employed in the next stage without purification.

후처리

  1. temperatureAfter the reaction solution has cooled to room temperature
  2. extractionextracted with diethyl ether
  3. customdried
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-78dffd7fbf1448c6b592c6e780722389
출처 데이터셋
uspto-grants-2004_01
특허 번호
US06677324B1

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