4-Chlorophenol → 1-(4-Chlorophenoxy)-2-chloro-2-propene

HRID 52308

반응식

HRID 52308 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[Cl:15][C:16]([CH2:18]Cl)=[CH2:17]>CC(C)=O>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH2:18][C:16]([Cl:15])=[CH2:17])=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 46844-ChlorophenolHCID 65652,3-DichloropropeneHCID 11430Potassium Carbonate

생성물 1

HCID 122548641-(4-Chlorophenoxy)-2-chloro-2-propene수율 98%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

To a mixture of 4-chlorophenol (6.1 g, 47.4 mmol) and potassium carbonate (13.1 g, 94.7 mmol) in acetone (200 mL), 2,3-dichloropropene (6.6 mL, 71 mmol) was added. After heating to reflux the reaction mixture for 48 hours, the reaction mixture was cooled and filtered. The residue was washed with more acetone and the combined filtrates were concentrated in vacuo. The crude pale brown liquid (11.5 g) was chromatographed (silica gel, hexane/ethyl acetate, 85/15) to give 1-(4-chlorophenoxy)-2-chloro-2-propene (8.9 g, 98%) as a white liquid: Anal. Calc'd. for C9H8OCl2 : C, 53.23, H, 3.97. Found: C, 53.09, H, 3.95.

후처리

  1. additionwas added
  2. temperatureAfter heating
  3. temperatureto reflux the reaction mixture for 48 hours
  4. temperaturethe reaction mixture was cooled
  5. filtrationfiltered
  6. washThe residue was washed with more acetone
  7. concentrationthe combined filtrates were concentrated in vacuo
  8. customThe crude pale brown liquid (11.5 g) was chromatographed (silica gel, hexane/ethyl acetate, 85/15)

출처 및 근거

ORD 기록
ord-d86c6284680f4dd89004ee407d378b0c
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05616601

연결된 노트

불러오는 중…