Boron Trichloride → Raloxifene Bismethyl Ether (hydrochloride)

HRID 50865

反応式

HRID 50865 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

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

後処理

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

出典と根拠

ORDレコード
ord-35e3eb27375e43f0be23b39b8d7563a3
出典データセット
uspto-grants-2004_03
特許番号
US06713494B1

関連ノート

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