Fluticasone → Fluticasone Propionate

HRID 1272567노트

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HRID 1272567 반응식
[CH3:1][C@H:2]1[C@:19]([OH:25])([C:20]([S:22][CH2:23][F:24])=[O:21])[C@:18]2([CH3:26])[C@H:4]([C@H:5]3[C@:15]([F:28])([C@@H:16]([OH:27])[CH2:17]2)[C@:14]2([CH3:29])[C:8](=[CH:9][C:10]([CH:12]=[CH:13]2)=[O:11])[C@@H:7]([F:30])[CH2:6]3)[CH2:3]1>CO.ClCCl>[CH3:8][CH2:9][C:10]([O:25][C@@:19]1([C:20]([S:22][CH2:23][F:24])=[O:21])[C@@:18]2([CH3:26])[CH2:17][C@H:16]([OH:27])[C@:15]3([F:28])[C@:14]4([CH3:29])[C:8](=[CH:9][C:10]([CH:12]=[CH:13]4)=[O:11])[C@@H:7]([F:30])[CH2:6][C@H:5]3[C@@H:4]2[CH2:3][C@H:2]1[CH3:1])=[O:11]

참가 물질

4

반응물 1

HCID 5311101Fluticasone

생성물 1

HCID 444036Fluticasone Propionate수율 155.9%

시약·촉매·용매 2

HCID 887Methanol용매HCID 6344Dichloromethane용매

실험 절차

The fluticasone (4.66 kg) obtained as above is dissolved in mixture of methanol (45 lit) and dichloromethane (45 lit) under stirring at ambient temperature and charcoalized. The methylene chloride is recovered (by distillation) by distillation at atmospheric pressure. The mixture is then gradually cooled to 10° C. and stirred for 60 min. The crystallized product is filtered, washed with methanol (4.5 lit) and dried at 55–60° C. to obtain pure fluticasone propionate (Yield 4.09 kg, overall yield 84.51%, purity 99.37%).

후처리

  1. customThe methylene chloride is recovered
  2. distillation(by distillation)
  3. distillationby distillation at atmospheric pressure
  4. temperatureThe mixture is then gradually cooled to 10° C.
  5. stirringstirred for 60 min
  6. filtrationThe crystallized product is filtered
  7. washwashed with methanol (4.5 lit)
  8. customdried at 55–60° C.

출처 및 근거

ORD 기록
ord-e7f874c5d0ed44289fc50c03bf3e8939
출처 데이터셋
uspto-grants-2007_04
특허 번호
US07208613B2

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