홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Methyl chloroformate → methyl N-[4-[4-(6-chloronaphthalen-2-yl)sulfonylpiperazine-1-carbonyl]benzenecarboximidoyl]carbamate

HRID 278605
노트
인쇄 미리보기

반응식

HRID 278605 반응식
Cl.[Cl:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[CH:9]=[C:8]([S:13]([N:16]1[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]1)(=[O:15])=[O:14])[CH:7]=[CH:6]2.C(N(CC)CC)C.Cl.[C:30]([C:33]1[CH:41]=[CH:40][C:36]([C:37](Cl)=[O:38])=[CH:35][CH:34]=1)(=[NH:32])[NH2:31].Cl[C:43]([O:45][CH3:46])=[O:44]>ClCCl.CN(C=O)C>[Cl:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[CH:9]=[C:8]([S:13]([N:16]1[CH2:17][CH2:18][N:19]([C:37](=[O:38])[C:36]3[CH:40]=[CH:41][C:33]([C:30](=[NH:32])[NH:31][C:43]([O:45][CH3:46])=[O:44])=[CH:34][CH:35]=3)[CH2:20][CH2:21]1)(=[O:14])=[O:15])[CH:7]=[CH:6]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6586Methyl chloroformateHCID 8471TriethylamineHCID 226280844-Amidinobenzoylchloride hydrochlorideHCID 227097661-(6-Chloronaphth-2-ylsulphonyl)piperazine hydrochloride

생성물 1

HCID 145840733methyl N-[4-[4-(6-chloronaphthalen-2-yl)sulfonylpiperazine-1-carbonyl]benzenecarboximidoyl]carbamate수율 19.3%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매

실험 절차

To a solution of 1-(6-chloronaphthalene-2-sulfonyl)piperazine hydrochloride (143 mg) and triethylamine (208 mg) in dichloromethane (10 ml) was added 4-amidinobenzoylchloride hydrochloride (108 mg), and the solution was stirred at room temperature for 1 hour, to which were added DMF (10 ml) and methyl chloroformate (200 mg). The solution was stirred at 50° C. for 30 minutes and the reaction solution was concentrated . The residue was dissolved in ethyl acetate, washed with water and sodium chloride solution, dried and concentrated. The residue was purified with silica gel column chromatography (ethyl acetate/methanol=40:1) to give colorless crystals of the title compound (41 mg).

후처리

  1. stirringThe solution was stirred at 50° C. for 30 minutes
  2. concentrationthe reaction solution was concentrated
  3. dissolutionThe residue was dissolved in ethyl acetate
  4. washwashed with water and sodium chloride solution
  5. customdried
  6. concentrationconcentrated
  7. customThe residue was purified with silica gel column chromatography (ethyl acetate/methanol=40:1)

출처 및 근거

ORD 기록
ord-534365849e7048628c5e463a043d2464
출처 데이터셋
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06359134B1

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트