Water → N-(5-Chloropyridin-2-yl)-2-[[4-(4-pyridinyl)piperazin-1-ylmethylcarbonyl]amino]benzamide

HRID 1247044

반응식

HRID 1247044 반응식
Br[CH2:2][C:3]([NH:5][C:6]1[CH:21]=[CH:20][CH:19]=[CH:18][C:7]=1[C:8]([NH:10][C:11]1[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][N:12]=1)=[O:9])=[O:4].C(=O)([O-])[O-].[K+].[K+].[N:28]1[CH:33]=[CH:32][C:31]([N:34]2[CH2:39][CH2:38][NH:37][CH2:36][CH2:35]2)=[CH:30][CH:29]=1.O>ClCCl>[Cl:17][C:14]1[CH:15]=[CH:16][C:11]([NH:10][C:8](=[O:9])[C:7]2[CH:18]=[CH:19][CH:20]=[CH:21][C:6]=2[NH:5][C:3]([CH2:2][N:37]2[CH2:38][CH2:39][N:34]([C:31]3[CH:32]=[CH:33][N:28]=[CH:29][CH:30]=3)[CH2:35][CH2:36]2)=[O:4])=[N:12][CH:13]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 705171-(4-Pyridyl)piperazineHCID 219063592-(Bromoacetyl)amino-N-(5-chloropyridin-2-yl)benzamide

생성물 1

HCID 21906548N-(5-Chloropyridin-2-yl)-2-[[4-(4-pyridinyl)piperazin-1-ylmethylcarbonyl]amino]benzamide수율 17.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 2-(bromoacetyl)amino-N-(5-chloropyridin-2-yl)benzamide (0.369 g, 1 mmol) in dichloromethane (10 ml) was added potassium carbonate (0.169 g, 1.22 mmol) and 1-(4-pyridyl)piperazine (0.171 mg, 1.05 mmol). The reaction was stirred overnight at room temperature. Water (2 mL) was added and the mixture was passed through a column of flux-calcined, high purity, inert diatomaceous earth packed into a polypropylene tube (article number CE 1103 from Varian) to remove water. The solvent was removed and the residue was purified by RPHPLC (CH2Cl2/5% 2 N ammonia in methanol) to give 0.08 g of pure title product.

후처리

  1. custompacked into a polypropylene tube
  2. custom(article number CE 1103 from Varian) to remove water
  3. customThe solvent was removed
  4. customthe residue was purified by RPHPLC (CH2Cl2/5% 2 N ammonia in methanol)

출처 및 근거

ORD 기록
ord-953b055c83b84ae3ab0500bdd498fc75
출처 데이터셋
uspto-grants-2006_10
특허 번호
US07129245B2

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