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

4-Toluenesulfonyl chloride → Ethyl 5,8-dimethyl-9-p-toluenesulfonylcarbazole-4-carboxylate

HRID 1197171
노트
인쇄 미리보기

반응식

HRID 1197171 반응식
[H-].[Na+].[CH3:3][C:4]1[CH:16]=[CH:15][C:14]([CH3:17])=[C:13]2[C:5]=1[C:6]1[C:7]([C:18]([O:20][CH2:21][CH3:22])=[O:19])=[CH:8][CH:9]=[CH:10][C:11]=1[NH:12]2.[C:23]1([CH3:33])[CH:28]=[CH:27][C:26]([S:29](Cl)(=[O:31])=[O:30])=[CH:25][CH:24]=1>CN(C)C=O>[CH3:3][C:4]1[CH:16]=[CH:15][C:14]([CH3:17])=[C:13]2[C:5]=1[C:6]1[C:7]([C:18]([O:20][CH2:21][CH3:22])=[O:19])=[CH:8][CH:9]=[CH:10][C:11]=1[N:12]2[S:29]([C:26]1[CH:27]=[CH:28][C:23]([CH3:33])=[CH:24][CH:25]=1)(=[O:31])=[O:30]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 73974-Toluenesulfonyl chlorideHCID 24758Sodium hydrideHCID 19897884Ethyl 5,8-dimethylcarbazole-4-carboxylate

생성물 1

HCID 19897871Ethyl 5,8-dimethyl-9-p-toluenesulfonylcarbazole-4-carboxylate수율 67%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매3회

실험 절차

To a suspension of 1.47 g of 60% sodium hydride (in a oil) in 35 ml of dry N,N-dimethylformamide was added dropwise over a 30 minutes period a solution of 7.00 g of ethyl 5,8-dimethylcarbazole-4-carboxylate obtained above in 35 ml of dry N,N-dimethylformamide, and the mixture was stirred for a further 30 minutes. To the mixture was added dropwise a solution of 6.99 g of p-toluenesulfonyl chloride in 35 ml of dry N,N-dimethyl-formamide, and the mixture was stirred further overnight. The reaction solution was poured into ice water and extracted with ethyl acetate, and the organic layer was washed, in turn, with dilute hydrochloric acid, a saturated aqueous sodium bicarbonate solution and a saturated aqueous sodium chloride solution, and dried over anhydrous magnesium sulfate. The solvent was evaporated, and the residue was chromatographed on silica gel column with hexane - ethyl acetate (9 : 1) to give 7.40 g of ethyl 5,8-dimethyl-9-p-toluenesulfonylcarbazole-4- carboxylate.

후처리

  1. stirringthe mixture was stirred further overnight
  2. extractionextracted with ethyl acetate
  3. washthe organic layer was washed, in turn, with dilute hydrochloric acid
  4. dry with materiala saturated aqueous sodium bicarbonate solution and a saturated aqueous sodium chloride solution, and dried over anhydrous magnesium sulfate
  5. customThe solvent was evaporated
  6. customthe residue was chromatographed on silica gel column with hexane - ethyl acetate (9 : 1)

출처 및 근거

ORD 기록
ord-20bd1d5fe80b462ea253b9837e149a0f
출처 데이터셋
uspto-grants-1992_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05116995

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트