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

Dimethyl Disulfide → Methyl 4,7-dimethyl-3-methylsulfenylindole-2-carboxylate

HRID 361623
노트
인쇄 미리보기

반응식

HRID 361623 반응식
CS[S:3][CH3:4].S(Cl)(Cl)(=O)=O.[CH3:10][C:11]1[CH:19]=[CH:18][C:17]([CH3:20])=[C:16]2[C:12]=1[CH:13]=[C:14]([C:21]([O:23][CH3:24])=[O:22])[NH:15]2>ClCCCl.CN(C=O)C.C(OCC)(=O)C>[CH3:10][C:11]1[CH:19]=[CH:18][C:17]([CH3:20])=[C:16]2[C:12]=1[C:13]([S:3][CH3:4])=[C:14]([C:21]([O:23][CH3:24])=[O:22])[NH:15]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 12232Dimethyl DisulfideHCID 24648Sulfuryl chlorideHCID 4714976methyl 4,7-dimethyl-1H-indole-2-carboxylate

생성물 1

HCID 53833292Methyl 4,7-dimethyl-3-methylsulfenylindole-2-carboxylate수율 105.1%

시약·촉매·용매 3

HCID 111,2-Dichloroethane용매HCID 6228
Dimethylformamide
용매
HCID 8857Ethyl Acetate용매

실험 절차

Under ice-cooling, 0.89 ml (7.4 mmol) of dimethyl disulfide was dissolved in 20 ml of 1,2-dichloroethane, and 0.53 ml (6.5 mmol) of sulfuryl chloride was added. The reaction mixture was stirred for 20 minutes and a solution of 2.00 g (9.8 imnol) of methyl 4,7-dimethylindole-2-carboxylate in 10 ml of anhydrous DMF was added. The reaction mixture was stirred for 2 hours, then dissolved in ethyl acetate and washed with water. The ethyl acetate layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography to provide 1.94 g of white crystals. Yield: 80%

후처리

  1. temperatureUnder ice-cooling
  2. stirringThe reaction mixture was stirred for 2 hours
  3. washwashed with water
  4. dry with materialThe ethyl acetate layer was dried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-5ecd86f17f7a45298e3846f5b76a82a7
출처 데이터셋
uspto-grants-1999_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05866594

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트