Ammonia → Oseltamivir

HRID 15606

反応式

HRID 15606 の反応式
[CH3:1][CH2:2][CH:3]([O:6][C@H:7]1[C@H:12]([NH:13][C:14]([CH3:16])=[O:15])[C@@H:11]([NH2:17])[CH2:10][C:9]([C:18]([O:20][CH2:21][CH3:22])=[O:19])=[CH:8]1)[CH2:4][CH3:5].OP(O)(O)=O.O.N>C(Cl)Cl>[CH3:5][CH2:4][CH:3]([O:6][C@H:7]1[C@H:12]([NH:13][C:14]([CH3:16])=[O:15])[C@@H:11]([NH2:17])[CH2:10][C:9]([C:18]([O:20][CH2:21][CH3:22])=[O:19])=[CH:8]1)[CH2:2][CH3:1]

参加物

5

反応物 3

HCID 222AmmoniaHCID 962WaterHCID 78000Tamiflu

生成物 1

HCID 65028Oseltamivir収率 108.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Oseltamivir phosphate (20 gm, HPLC purity: 97%) is stirred with water (100 ml) and methylene chloride (100 ml) for 10 minutes at 25-30° C. and then pH of the mass is adjusted to 9-10 with liquor ammonia. Separated the layers, the organic layer is subjected to carbon treatment and filtered on hiflo bed. Washed the hiflo bed with methylene chloride (20 ml) and then distilled the organic layer under vacuum at 40° C. to give 16.5 gm of oseltamivir free base as a residue.

後処理

  1. customSeparated the layers
  2. filtrationfiltered on hiflo bed
  3. washWashed the hiflo bed with methylene chloride (20 ml)
  4. distillationdistilled the organic layer under vacuum at 40° C.

出典と根拠

ORDレコード
ord-950cdd41c55d4453b1774526ef2cfe7b
出典データセット
uspto-grants-2010_06
特許番号
US07732632B2

関連ノート

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