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

Dimethyl Sulfoxide → 6-(2,6-Dichlorophenyl)-8-methyl-2-methylsulfonyl-8H-pyrido[2,3-d]pyrimidin-7-one

HRID 3181
노트
인쇄 미리보기

반응식

HRID 3181 반응식
ClC1C=CC=C(C(OO)=[O:9])C=1.[Cl:12][C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([Cl:19])[C:14]=1[C:20]1[C:31](=[O:32])[N:30]([CH3:33])[C:23]2[N:24]=C(SC)[N:26]=[CH:27][C:22]=2[CH:21]=1.[CH3:34][S:35]([CH3:37])=[O:36]>C(Cl)(Cl)Cl>[Cl:12][C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([Cl:19])[C:14]=1[C:20]1[C:31](=[O:32])[N:30]([CH3:33])[C:23]2[N:24]=[C:34]([S:35]([CH3:37])(=[O:9])=[O:36])[N:26]=[CH:27][C:22]=2[CH:21]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 679Dimethyl SulfoxideHCID 70297m-Chloroperbenzoic acidHCID 107367016-(2,6-Dichlorophenyl)-8-methyl-2-(methylthio)pyrido[2,3-d]pyrimidin-7(8H)-one

생성물 1

HCID 105961576-(2,6-Dichlorophenyl)-8-methyl-2-methylsulfonyl-8H-pyrido[2,3-d]pyrimidin-7-one

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

A quantity of 0.346 g (1.00 mmol) of 50% to 60% m-chloroperbenzoic acid (assuming 50% peracid was present) was added at 25° C. to a stirred solution of 0.165 g (0.47 mmol) of 6-(2,6-dichlorophenyl)-8-methyl-2-methylsulfanyl-8H-pyrido[2,3-d]pyrimidin-7-one of Example 37 in 15 mL of chloroform, and the solution was stirred overnight. A quantity of 0.25 g (3.20 mmol) of dimethylsulfoxide was added to reduce any excess peracid. After 15 minutes, the chloroform solution was washed with 30 mL of saturated sodium bicarbonate and then with water. The separated organic layer was dried over sodium sulfate, filtered, and concentrated to ca. 5 mL volume. Crystals separated. Added ca. 5 mL of petroleum ether and filtered; wt 0.165 g (92%); mp >290° C.

후처리

  1. waitAfter 15 minutes
  2. washthe chloroform solution was washed with 30 mL of saturated sodium bicarbonate
  3. dry with materialThe separated organic layer was dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated to ca. 5 mL volume
  6. customCrystals separated
  7. additionAdded ca. 5 mL of petroleum ether
  8. filtrationfiltered

출처 및 근거

ORD 기록
ord-bfb87e53646f4c08bf6331ebf2a578a0
출처 데이터셋
uspto-grants-1998_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05733914

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트