Bazedoxifene Acetate → Bazedoxifene

HRID 1503317

反応式

HRID 1503317 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>CS(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 94%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

反応条件

温度
65 °C

実験手順

Bazedoxifene acetate (3 g) and dimethylsulfoxide (15 mL) are mixed and heated to 60-70° C. to produce a clear solution, followed by cooling to room temperature and filtration to make it particle free. To the filtrate, toluene (150 mL), 10% aqueous sodium carbonate solution (5 mL) and water (75 mL) are added and the mixture is stirred at room temperature for solid formation. The solid so formed is collected by filtration, washed with toluene (6 mL), water (6 mL) and dried under vacuum below 80° C. for about 7 hours to afford 2.5 g of crystalline bazedoxifene free base Form A.

後処理

  1. customto produce a clear solution
  2. temperatureby cooling to room temperature
  3. filtrationfiltration
  4. additionTo the filtrate, toluene (150 mL), 10% aqueous sodium carbonate solution (5 mL) and water (75 mL) are added
  5. customThe solid so formed
  6. filtrationis collected by filtration
  7. washwashed with toluene (6 mL), water (6 mL)
  8. customdried under vacuum below 80° C. for about 7 hours

出典と根拠

ORDレコード
ord-0616b5f881544275bb673f0cc2cd4451
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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