Boron tribromide → N-{2-[4-(3,4-Dichlorophenoxy)-1-piperidinyl]ethyl}-3-hydroxybenzamide hydrochloride

HRID 496876노트

반응식

HRID 496876 반응식
Cl.[Cl:2][C:3]1[CH:4]=[C:5]([CH:26]=[CH:27][C:28]=1[Cl:29])[O:6][CH:7]1[CH2:12][CH2:11][N:10]([CH2:13][CH2:14][NH:15][C:16](=[O:25])[C:17]2[CH:22]=[CH:21][CH:20]=[C:19]([O:23]C)[CH:18]=2)[CH2:9][CH2:8]1.B(Br)(Br)Br>ClCCl>[ClH:2].[Cl:2][C:3]1[CH:4]=[C:5]([CH:26]=[CH:27][C:28]=1[Cl:29])[O:6][CH:7]1[CH2:12][CH2:11][N:10]([CH2:13][CH2:14][NH:15][C:16](=[O:25])[C:17]2[CH:22]=[CH:21][CH:20]=[C:19]([OH:23])[CH:18]=2)[CH2:9][CH2:8]1

참가 물질

4

반응물 2

HCID 25134Boron tribromideHCID 22322410N-{2-[4-(3,4-Dichlorophenoxy)-1-piperidinyl]ethyl}-3-methoxybenzamide hydrochloride

생성물 1

HCID 22322198N-{2-[4-(3,4-Dichlorophenoxy)-1-piperidinyl]ethyl}-3-hydroxybenzamide hydrochloride수율 137.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

The product of Example 10 (0.15 g) was dissolved in dichloromethane (10 ml) and a solution of 1.0M BBr3 in dichloromethane (4 ml) added. After 16 hours at room temperature the solvent was removed by evaporation, methanol was added and the solution concentrated. The residue was dissolved in 2M aqueous HCl solution, concentrated to dryness and the residue triturated under ether to give the titled product as a solid (0.1 g).

후처리

  1. customAfter 16 hours at room temperature the solvent was removed by evaporation, methanol
  2. additionwas added
  3. concentrationthe solution concentrated
  4. dissolutionThe residue was dissolved in 2M aqueous HCl solution
  5. concentrationconcentrated to dryness
  6. customthe residue triturated under ether

출처 및 근거

ORD 기록
ord-909116f1b5e34b13aa55e6ba8a663aa5
출처 데이터셋
uspto-grants-2005_09
특허 번호
US06946478B2

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