Boron Trichloride → Raloxifene Bismethyl Ether (hydrochloride)

HRID 50865

반응식

HRID 50865 반응식
B(Cl)(Cl)[Cl:2].[CH3:5][O:6][C:7]1[CH:8]=[CH:9][C:10]2[C:14]([C:15](=[O:31])[C:16]3[CH:21]=[CH:20][C:19]([O:22][CH2:23][CH2:24][N:25]4[CH2:30][CH2:29][CH2:28][CH2:27][CH2:26]4)=[CH:18][CH:17]=3)=[C:13]([C:32]3[CH:37]=[CH:36][C:35]([O:38][CH3:39])=[CH:34][CH:33]=3)[S:12][C:11]=2[CH:40]=1>C(Cl)Cl>[ClH:2].[CH3:5][O:6][C:7]1[CH:8]=[CH:9][C:10]2[C:14]([C:15](=[O:31])[C:16]3[CH:17]=[CH:18][C:19]([O:22][CH2:23][CH2:24][N:25]4[CH2:26][CH2:27][CH2:28][CH2:29][CH2:30]4)=[CH:20][CH:21]=3)=[C:13]([C:32]3[CH:37]=[CH:36][C:35]([O:38][CH3:39])=[CH:34][CH:33]=3)[S:12][C:11]=2[CH:40]=1

참가 물질

4

반응물 2

HCID 25135Boron TrichlorideHCID 10767755Raloxifene Bismethyl Ether

생성물 1

HCID 45260096Raloxifene Bismethyl Ether (hydrochloride)

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of the compound prepared as described in Preparation 1 (8.46 grams) and the acid chloride prepared as described in Preparation 3 (10.0 grams) in methylene chloride (350 mL) was cooled:to about 20-25° C. The cool mixture was treated with boron trichloride (2.6 mL), and the resulting mixture mechanically stirred. The reaction was monitored by HPLC using the assay described above. After 85 minutes, the in situ HPLC yield based on a 6-methoxy-2-(4-methoxyphenyl)-3-[4-(2-piperidinylethoxy)benzoyl]benzo[b]thiophene standard was 88%.

후처리

  1. additionA mixture of the compound
  2. customprepared
  3. temperaturewas cooled
  4. customto about 20-25° C
  5. customthe in situ HPLC yield

출처 및 근거

ORD 기록
ord-35e3eb27375e43f0be23b39b8d7563a3
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06713494B1

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