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

HRID 989804

반응식

HRID 989804 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

반응 조건

온도
35 °C

실험 절차

A solution of 6-methoxy-2-(4-methoxyphenyl)-3-[4-(2-piperidinoethoxy)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 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.

후처리

  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. waitAfter one hour
  6. filtrationthe crystalline product was filtered
  7. washwashed with cold ethanol (10 mL)
  8. customdried at 40° C. in vacuo

출처 및 근거

ORD 기록
ord-e8ea92b8528041f484958dbcbab02358
출처 데이터셋
uspto-grants-2002_10
특허 번호
US06458811B1

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