tert-Butyl methyl ether → Bazedoxifene Acetate

HRID 1503318

반응식

HRID 1503318 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.[C:36]([O:40]C)([CH3:39])(C)C>C(O)(=O)C>[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.[CH3:39][C:36]([OH:40])=[O:17]

참가 물질

4

반응물 2

HCID 15413tert-Butyl methyl etherHCID 154257Bazedoxifene

생성물 1

HCID 154256Bazedoxifene Acetate

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

Bazedoxifene free base (400 mg) and methyl tert-butyl ether (30 mL) are mixed and stirred for about 10 minutes. Acetic acid (0.17 g) is added slowly through a dropper and the mixture is stirred overnight for solid formation. The solid is collected by filtration to afford 250 mg of crystalline bazedoxifene acetate Form D.

후처리

  1. stirringthe mixture is stirred overnight for solid formation
  2. filtrationThe solid is collected by filtration

출처 및 근거

ORD 기록
ord-b6ac894438f44dbcbe6c1b754deae012
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09212172B2

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