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

Saccharin → 2-(1,3-Benzodioxol-5-ylmethyl)-1,1-dioxo-1,2-benzothiazol-3-one

HRID 1449537
노트
인쇄 미리보기

반응식

HRID 1449537 반응식
[S:1]1([C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[C:5](=[O:6])[NH:4]1)(=[O:3])=[O:2].[CH2:13]1[O:23][C:22]2[CH:21]=[CH:20][C:17]([CH2:18]Cl)=[CH:16][C:15]=2[O:14]1>CN(C=O)C.C(Cl)Cl.C(OCC)(=O)C>[O:23]1[C:22]2[CH:21]=[CH:20][C:17]([CH2:18][N:4]3[C:5](=[O:6])[C:7]4[CH:8]=[CH:9][CH:10]=[CH:11][C:12]=4[S:1]3(=[O:2])=[O:3])=[CH:16][C:15]=2[O:14][CH2:13]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 5143SaccharinHCID 887131,3-Benzodioxole, 5-(chloromethyl)-

생성물 1

HCID 64639312-(1,3-Benzodioxol-5-ylmethyl)-1,1-dioxo-1,2-benzothiazol-3-one

시약·촉매·용매 3

HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매2회HCID 8857Ethyl Acetate
용매

실험 절차

To saccharin (5.0 g, 0.0273 mol) in DMF (10 mL) was added Nail (1.15 g, 60% in oil, 0.0288 mol) with ice bath cooling. After stirring for 10 minutes. a solution of 3,4-methylenedioxybenzyl chloride in methylene chloride, 50% by weight, (10 g, 0.0293 mol) was added and the mixture stirred for 16 hours. The mixture was diluted with ethyl acetate (200 mL) containing 10% methylene chloride and washed with IN HCl (2×100 mL). The organic phase was washed with brine and dried over MgSO4. The mixture was concentrated until crystals were apparent. After standing for 16 hours the product was collected by filtration (4.2 g, 49%);

후처리

  1. temperaturecooling
  2. stirringthe mixture stirred for 16 hours
  3. washwashed with IN HCl (2×100 mL)
  4. washThe organic phase was washed with brine
  5. dry with materialdried over MgSO4
  6. concentrationThe mixture was concentrated until crystals
  7. waitAfter standing for 16 hours
  8. filtrationthe product was collected by filtration (4.2 g, 49%)

출처 및 근거

ORD 기록
ord-f9e46906a401421eb678aa1853c7cd2d
출처 데이터셋
uspto-grants-1997_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05599811

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트