Potassium Carbonate → tert-Butyl 4-(3-((6-chloro-2-naphthyl)sulfonyl)propanoyl)-3-(2-ethoxy-2-oxoethyl)piperazine-1-carboxylate

HRID 493708노트

반응식

HRID 493708 반응식
[CH2:1]([O:3][C:4](=[O:19])[CH2:5][CH:6]1[NH:11][CH2:10][CH2:9][N:8]([C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[CH2:7]1)[CH3:2].[Cl:20][C:21]1[CH:22]=[C:23]2[C:28](=[CH:29][CH:30]=1)[CH:27]=[C:26]([S:31]([CH2:34][CH2:35][C:36](O)=[O:37])(=[O:33])=[O:32])[CH:25]=[CH:24]2.C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C.C(=O)([O-])[O-].[K+].[K+]>ClCCl.C(N(CC)CC)C>[Cl:20][C:21]1[CH:22]=[C:23]2[C:28](=[CH:29][CH:30]=1)[CH:27]=[C:26]([S:31]([CH2:34][CH2:35][C:36]([N:11]1[CH2:10][CH2:9][N:8]([C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[CH2:7][CH:6]1[CH2:5][C:4]([O:3][CH2:1][CH3:2])=[O:19])=[O:37])(=[O:32])=[O:33])[CH:25]=[CH:24]2

참가 물질

8

반응물 5

HCID 11430Potassium CarbonateHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 111973043-(6-Chloro-2-naphthyl)sulfonylpropionic acidHCID 16114865tert-Butyl 3-(2-ethoxy-2-oxoethyl)piperazine-1-carboxylate

생성물 1

HCID 23130960tert-Butyl 4-(3-((6-chloro-2-naphthyl)sulfonyl)propanoyl)-3-(2-ethoxy-2-oxoethyl)piperazine-1-carboxylate수율 60.2%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8471Triethylamine용매

실험 절차

tert-Butyl 3-(2-ethoxy-2-oxoethyl)piperazine-1-carboxylate (0.9 g) was dissolved in dichloromethane (20 mL), and triethylamine (0.92 mL) was added thereto. With ice cooling, 3-((6-chloro-2-naphthyl)sulfonyl)propionic acid (1.0 g), HOBt (0.55 g) and WSC (0.65 g) were added thereto, and the mixture was mixed at room temperature for 16 hours. The reaction solution was basified with an aqueous potassium carbonate solution, then extracted with chloroform, and the extract was dried over anhydrous magnesium sulfate. The solvent was distilled off to give the title compound (1.1 g) as a pale brown oily matter.

후처리

  1. additionthe mixture was mixed at room temperature for 16 hours
  2. extractionextracted with chloroform
  3. dry with materialthe extract was dried over anhydrous magnesium sulfate
  4. distillationThe solvent was distilled off

출처 및 근거

ORD 기록
ord-5ca0fc94541246eca32edbf048bd455c
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07534887B2

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