Ethanol → 6-Hydroxy-2-(4-hydroxyphenyl)-3-(4-(2-piperidinoethoxy)-benzoyl]benzo[b]thiophene Hydrochloride 1,2-Dichloroethane

HRID 50866

反応式

HRID 50866 の反応式
[ClH:1].C[O:3][C:4]1[CH:5]=[CH:6][C:7]2[C:11]([C:12](=[O:28])[C:13]3[CH:18]=[CH:17][C:16]([O:19][CH2:20][CH2:21][N:22]4[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]4)=[CH:15][CH:14]=3)=[C:10]([C:29]3[CH:34]=[CH:33][C:32]([O:35]C)=[CH:31][CH:30]=3)[S:9][C:8]=2[CH:37]=1.B(Cl)(Cl)[Cl:39].C(O)C.CO>ClCCCl>[Cl:1][CH2:8][CH2:37][Cl:39].[ClH:39].[OH:3][C:4]1[CH:5]=[CH:6][C:7]2[C:11]([C:12](=[O:28])[C:13]3[CH:14]=[CH:15][C:16]([O:19][CH2:20][CH2:21][N:22]4[CH2:23][CH2:24][CH2:25][CH2:26][CH2:27]4)=[CH:17][CH:18]=3)=[C:10]([C:29]3[CH:30]=[CH:31][C:32]([OH:35])=[CH:33][CH:34]=3)[S:9][C:8]=2[CH:37]=1

参加物

6

反応物 4

HCID 702EthanolHCID 887MethanolHCID 25135Boron TrichlorideHCID 45260096Raloxifene Bismethyl Ether (hydrochloride)

生成物 1

HCID 99168796-Hydroxy-2-(4-hydroxyphenyl)-3-(4-(2-piperidinoethoxy)-benzoyl]benzo[b]thiophene Hydrochloride 1,2-Dichloroethane

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

反応条件

温度
35 °C

実験手順

A solution of 6-methoxy -2-(4-methoxyphenyl)-3-[4-(2-piperidinylethoxy)benzoyl]benzo[b]thiophene hydrochloride (2.0 g) in 1,2-dichloroethane (20 mL) was treated with boron trichloride (2.0 mL). The resulting mixture was stirred at 35° C. for about 18 hours. A:mixture of ethanol and methanol (10 mL, 95:5, 3A) was treated with the reaction mixture from above, causing the alcoholic mixture to reflux. Upon complete addition, the resulting crystalline slurry was stirred at 25° C. After one 1 hour, the crystalline product was filtered, washed with cold ethanol (10 mL), and dried at 40° C. in vacuo to give 1.78 g of the title compound. The X-ray powder diffraction pattern is identical to that reported in Table 1.

後処理

  1. additionwas treated with the reaction mixture from above,
  2. temperatureto reflux
  3. additionUpon complete addition
  4. stirringthe resulting crystalline slurry was stirred at 25° C
  5. filtrationAfter one 1 hour, the crystalline product was filtered
  6. washwashed with cold ethanol (10 mL)
  7. customdried at 40° C. in vacuo

出典と根拠

ORDレコード
ord-60db984ddf1c46718e7c16f6fef6eee1
出典データセット
uspto-grants-2004_03
特許番号
US06713494B1

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