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

HRID 1059016ノート

反応式

HRID 1059016 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-21d9a418f6b04a7d806c708bf18d9704
出典データセット
uspto-grants-2003_02
特許番号
US06518286B1

反応ノート

読み込み中…