Fluticasone → Fluticasone Propionate

HRID 1272567

反応式

HRID 1272567 の反応式
[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]

参加物

4

反応物 1

HCID 5311101Fluticasone

生成物 1

HCID 444036Fluticasone Propionate収率 155.9%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6344Dichloromethane溶媒

実験手順

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%).

後処理

  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.

出典と根拠

ORDレコード
ord-e7f874c5d0ed44289fc50c03bf3e8939
出典データセット
uspto-grants-2007_04
特許番号
US07208613B2

関連ノート

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