tert-Butyl methyl ether → Bazedoxifene Acetate

HRID 1503318

反応式

HRID 1503318 の反応式
[CH3:1][C:2]1[C:3]2[CH:4]=[C:5]([OH:35])[CH:6]=[CH:7][C:8]=2[N:9]([CH2:18][C:19]2[CH:20]=[CH:21][C:22]([O:25][CH2:26][CH2:27][N:28]3[CH2:34][CH2:33][CH2:32][CH2:31][CH2:30][CH2:29]3)=[CH:23][CH:24]=2)[C:10]=1[C:11]1[CH:12]=[CH:13][C:14]([OH:17])=[CH:15][CH:16]=1.[C:36]([O:40]C)([CH3:39])(C)C>C(O)(=O)C>[CH3:1][C:2]1[C:3]2[CH:4]=[C:5]([OH:35])[CH:6]=[CH:7][C:8]=2[N:9]([CH2:18][C:19]2[CH:24]=[CH:23][C:22]([O:25][CH2:26][CH2:27][N:28]3[CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34]3)=[CH:21][CH:20]=2)[C:10]=1[C:11]1[CH:12]=[CH:13][C:14]([OH:17])=[CH:15][CH:16]=1.[CH3:39][C:36]([OH:40])=[O:17]

参加物

4

反応物 2

HCID 15413tert-Butyl methyl etherHCID 154257Bazedoxifene

生成物 1

HCID 154256Bazedoxifene Acetate

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

Bazedoxifene free base (400 mg) and methyl tert-butyl ether (30 mL) are mixed and stirred for about 10 minutes. Acetic acid (0.17 g) is added slowly through a dropper and the mixture is stirred overnight for solid formation. The solid is collected by filtration to afford 250 mg of crystalline bazedoxifene acetate Form D.

後処理

  1. stirringthe mixture is stirred overnight for solid formation
  2. filtrationThe solid is collected by filtration

出典と根拠

ORDレコード
ord-b6ac894438f44dbcbe6c1b754deae012
出典データセット
uspto-grants-2015_12
特許番号
US09212172B2

関連ノート

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