Bazedoxifene Acetate → Bazedoxifene

HRID 1503313

反応式

HRID 1503313 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.CC(O)=O>CN(C)C=O>[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

参加物

3

反応物 1

HCID 154256Bazedoxifene Acetate

生成物 1

HCID 154257Bazedoxifene

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

Bazedoxifene acetate (47 g) and dimethylformamide (235 mL) are mixed and heated to 80° C. to produce a clear solution, followed by filtration. To the filtrate, toluene (2700 mL), morpholine (3.0 mL), and water (1810 mL) are added and the mixture is stirred overnight at room temperature. The solid is collected by filtration, washed with toluene (70 mL) and water (70 mL), then dried under vacuum below 80° C. for about 6-8 hours to afford Form A of crystalline bazedoxifene free base: D90=49.80 microns; D10=3.61 microns, D50=25.30 microns. The material is subjected to micronization under nitrogen atmosphere with a pressure of 4 kg/cm2 to afford the particles with D90=6.04 microns; D10=0.89 microns, D50=2.37 microns.

後処理

  1. customto produce a clear solution
  2. filtrationfollowed by filtration
  3. additionTo the filtrate, toluene (2700 mL), morpholine (3.0 mL), and water (1810 mL) are added
  4. filtrationThe solid is collected by filtration
  5. washwashed with toluene (70 mL) and water (70 mL)
  6. customdried under vacuum below 80° C. for about 6-8 hours

出典と根拠

ORDレコード
ord-eff699e8967c46adb4b8550d94e716c7
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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