Bazedoxifene Acetate → Bazedoxifene

HRID 1503317

반응식

HRID 1503317 반응식
[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

참가 물질

3

반응물 1

HCID 154256Bazedoxifene Acetate

생성물 1

HCID 154257Bazedoxifene수율 94%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

반응 조건

온도
65 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0616b5f881544275bb673f0cc2cd4451
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09212172B2

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