Boron Trichloride → Raloxifene Bismethyl Ether (hydrochloride)

HRID 989803

反応式

HRID 989803 の反応式
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

参加物

4

反応物 2

HCID 25135Boron TrichlorideHCID 10767755Raloxifene Bismethyl Ether

生成物 1

HCID 45260096Raloxifene Bismethyl Ether (hydrochloride)

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
22.5 °C

実験手順

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-piperidinoethoxy)benzoyl]benzo[b]thiophene standard was 88%.

後処理

  1. additionA mixture of the compound
  2. customprepared
  3. customthe in situ HPLC yield

出典と根拠

ORDレコード
ord-1e25909ca3c341a2bdb0cddc8aeb31ff
出典データセット
uspto-grants-2002_10
特許番号
US06458811B1

関連ノート

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