Bazedoxifene Acetate → Bazedoxifene

HRID 1503313

반응식

HRID 1503313 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 154257Bazedoxifene

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-eff699e8967c46adb4b8550d94e716c7
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09212172B2

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