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

4-Chlorophenol → HCID 14328588, 화합물

HRID 1087699
노트
인쇄 미리보기

반응식

HRID 1087699 반응식
Cl[CH2:2][C:3](=[O:10])[C:4]([CH3:9])([CH3:8])[CH:5]([CH3:7])[CH3:6].[Cl:11][C:12]1[CH:17]=[CH:16][C:15]([OH:18])=[CH:14][CH:13]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[Cl:11][C:12]1[CH:17]=[CH:16][C:15]([O:18][CH2:2][C:3](=[O:10])[C:4]([CH3:9])([CH3:8])[CH:5]([CH3:7])[CH3:6])=[CH:14][CH:13]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 46844-ChlorophenolHCID 11430Potassium CarbonateHCID 132952261-Chloro-3,3,4-trimethylpentan-2-one

생성물 1

HCID 14328588HCID 14328588, 화합물수율 87.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
100 °C

실험 절차

461.5 9 (2.84 mols) of 1-chloro-3,3,4-trimethylpentan-2-one are added with stirring over the course of 1 hour to a mixture of 364.9 g (2.84 mols of 4-chlorophenol and 392 g (2.84 mols of potassium carbonate heated to 100° C. in 2,700 ml of N,N-dimethylformamide. After heating at 100° C. for ten hours, the mixture is cooled to 20° C., precipitated potassium chloride is removed by filtration, and the filtrate is evaporated under reduced pressure. The residue is taken up in 1,500 ml of dichloromethane and washed twice with 750 ml of 5% strength aqueous sodium hydroxide solution and 750 ml of water each time. After drying the organic phase over anhydrous sodium sulphate, the solvent is removed by distillation under reduced pressure and the oily residue is distilled in vacuo. 632 g (87.4% of theory) of 1-(4-chlorophenoxy)-3,3,4-trimethylpentan-2-one of boiling point 147°-148° C./0.15 torr are thus obtained.

후처리

  1. temperaturethe mixture is cooled to 20° C.
  2. customprecipitated potassium chloride
  3. customis removed by filtration
  4. customthe filtrate is evaporated under reduced pressure
  5. washwashed twice with 750 ml of 5% strength aqueous sodium hydroxide solution and 750 ml of water each time
  6. dry with materialAfter drying the organic phase over anhydrous sodium sulphate
  7. customthe solvent is removed by distillation under reduced pressure
  8. distillationthe oily residue is distilled in vacuo

출처 및 근거

ORD 기록
ord-c01771d9d7854c478097b613c2f82c4c
출처 데이터셋
uspto-grants-1990_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04960453

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트