Bazedoxifene Acetate → Bazedoxifene

HRID 1503311

반응식

HRID 1503311 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>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

참가 물질

3

반응물 1

HCID 154256Bazedoxifene Acetate

생성물 1

HCID 154257Bazedoxifene수율 75.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
72.5 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-26db185c049d42e98fd7a3967d07ba63
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09212172B2

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