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

Dimethyl Sulfide → 6-(6-Bromo-5-nitroso-3-phenyl-2-pyrazinyl)-2-isopropyl-3(2h)-pyridazinone

HRID 915051
노트
인쇄 미리보기

반응식

HRID 915051 반응식
ClC1C=CC=C(C(OO)=[O:9])C=1.[Br:12][C:13]1[N:18]=[C:17]([C:19]2[CH:20]=[CH:21][C:22](=[O:28])[N:23]([CH:25]([CH3:27])[CH3:26])[N:24]=2)[C:16]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)=[N:15][C:14]=1[N:35]=S(C)C.CSC.C([O-])([O-])=O.[Na+].[Na+]>C(Cl)Cl>[Br:12][C:13]1[N:18]=[C:17]([C:19]2[CH:20]=[CH:21][C:22](=[O:28])[N:23]([CH:25]([CH3:27])[CH3:26])[N:24]=2)[C:16]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)=[N:15][C:14]=1[N:35]=[O:9]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 1068Dimethyl SulfideHCID 10340Sodium CarbonateHCID 70297m-Chloroperbenzoic acidHCID 877986596-{6-bromo-5-[(dimethyl-lambda~4~-sulfanylidene)amino]-3-phenyl-2-pyrazinyl}-2-isopropyl-3 (2H)-pyridazinone

생성물 1

HCID 877873306-(6-Bromo-5-nitroso-3-phenyl-2-pyrazinyl)-2-isopropyl-3(2h)-pyridazinone수율 49.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of m-chloroperbenzoic acid (70-75% purity) (1.66 g) in CH2Cl2 (40 ml) was added a solution of 6-{6-bromo-5-[(dimethyl-lambda˜4˜-sulfanylidene)amino]-3-phenyl-2-pyrazinyl}-2-isopropyl-3 (2H)-pyridazinone (2.01 g) in CH2Cl2 (20 ml) at −10˜-5° C. and the mixture was stirred at the same temperature for one hour. After addition of dimethyl sulfide (0.25 ml), the solution was stirred at the same temperature for 30 minutes. Sat. aq. Na2CO3 (50 ml) was then added to the mixture. An organic layer was collected, dried over MgSO4, concentrated under reduced pressure and purified by column chromatography on silica gel eluting with a mixture of n-hexane and EtOAc (70:30 v/v) to give 6-(6-bromo-5-nitroso-3-phenyl-2-pyrazinyl)-2-isopropyl-3(2H)-pyridazinone as a solid (0.896 g).

후처리

  1. stirringthe solution was stirred at the same temperature for 30 minutes
  2. customAn organic layer was collected
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated under reduced pressure
  5. custompurified by column chromatography on silica gel eluting with a mixture of n-hexane and EtOAc (70:30 v/v)

출처 및 근거

ORD 기록
ord-d1997d09c60b4596949a9a39b9828b96
출처 데이터셋
uspto-grants-2007_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07265120B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트