Bazedoxifene Acetate → Bazedoxifene

HRID 1503311

反応式

HRID 1503311 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収率 75.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
72.5 °C

実験手順

Bazedoxifene acetate (15 g) and dimethylformamide (75 mL) are mixed and heated to 70-75° C. to produce a clear solution, followed by filtration to make it particle free. To the filtrate, toluene (1000 mL), morpholine (1 mL), and water (500 mL) are added and the mixture is cooled to 25-30° C. and stirred overnight. The solid that forms is collected by filtration, washed with toluene (20 mL), and dried under vacuum at 70° C. for 5 hours to afford 10 g of crystalline bazedoxifene free base Form A.

後処理

  1. customto produce a clear solution
  2. filtrationfollowed by filtration
  3. additionTo the filtrate, toluene (1000 mL), morpholine (1 mL), and water (500 mL) are added
  4. temperaturethe mixture is cooled to 25-30° C.
  5. filtrationThe solid that forms is collected by filtration
  6. washwashed with toluene (20 mL)
  7. customdried under vacuum at 70° C. for 5 hours

出典と根拠

ORDレコード
ord-26db185c049d42e98fd7a3967d07ba63
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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