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

Ethyl bromoacetate → HCID 22097159, 화합물

HRID 861498
노트
인쇄 미리보기

반응식

HRID 861498 반응식
[N+:1]([C:4]1[CH:13]=[C:12]([N+:14]([O-:16])=[O:15])[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]=1[NH:17][S:18]([C:21]1[CH:26]=[CH:25][C:24]([CH3:27])=[CH:23][CH:22]=1)(=[O:20])=[O:19])([O-:3])=[O:2].C([O-])(C)(C)C.[K+].Br[CH2:35][C:36]([O:38][CH2:39][CH3:40])=[O:37]>CN(C)C=O>[CH2:39]([O:38][C:36]([CH2:35][N:17]([C:5]1[C:6]2[C:11](=[CH:10][CH:9]=[CH:8][CH:7]=2)[C:12]([N+:14]([O-:16])=[O:15])=[CH:13][C:4]=1[N+:1]([O-:3])=[O:2])[S:18]([C:21]1[CH:26]=[CH:25][C:24]([CH3:27])=[CH:23][CH:22]=1)(=[O:20])=[O:19])=[O:37])[CH3:40]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7748Ethyl bromoacetateHCID 294498N-(2,4-Dinitro-1-naphthyl)-P-toluenesulfonamideHCID 23665647Potassium tert-butoxide

생성물 1

HCID 22097159HCID 22097159, 화합물수율 76%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

60 g (155 mmol) of N-(2,4-dinitro-1-naphthyl)-4-methylphenylsulfonamide (J. Soc. Chem. 1935, 1855) were dissolved in 500 ml of anhydrous dimethylformamide under protective gas and 19.1 g (170 mmol) of potassium tert-butanolate were added a little at a time. The mixture was stirred at room temperature for about 30 minutes, and then 25.9 g (155 mmol) of ethyl bromoacetate dissolved in 50 ml of anhydrous dimethylformamide were added dropwise. The mixture was then heated at 100° C. for 90 minutes and, after cooling, poured into ice-water, and the aqueous phase was extracted with ethyl acetate. The organic phase was dried and concentrated under reduced pressure. The residue was heated with a mixture of 50 ml of toluene and 100 ml of ethanol and the resulting crystals were filtered off with suction to yield 55.7 g (76%) of the product. Melting point 106°-107° C.

후처리

  1. additionwere added a little at a time
  2. additionwere added dropwise
  3. temperatureThe mixture was then heated at 100° C. for 90 minutes
  4. temperatureafter cooling
  5. extractionthe aqueous phase was extracted with ethyl acetate
  6. customThe organic phase was dried
  7. concentrationconcentrated under reduced pressure
  8. temperatureThe residue was heated with a mixture of 50 ml of toluene and 100 ml of ethanol
  9. filtrationthe resulting crystals were filtered off with suction

출처 및 근거

ORD 기록
ord-f40fdcd342e746b8aba1601cdf317c28
출처 데이터셋
uspto-grants-1998_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05714489

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트