1-Chloro-1,1-difluoro-5,5-dimethyl-2,4-hexanedione → 1-Chloro-1,1-difluoro-5,5-dimethyl-3-ethoxymethylene-2,4-hexanedione

HRID 964908노트

반응식

HRID 964908 반응식
[Cl:1][C:2]([F:13])([F:12])[C:3](=[O:11])[CH2:4][C:5](=[O:10])[C:6]([CH3:9])([CH3:8])[CH3:7].[CH:14]([O-])([O-])[O:15][CH2:16][CH3:17]>C(OC(=O)C)(=O)C>[Cl:1][C:2]([F:12])([F:13])[C:3](=[O:11])[C:4](=[CH:14][O:15][CH2:16][CH3:17])[C:5](=[O:10])[C:6]([CH3:9])([CH3:7])[CH3:8]

참가 물질

4

반응물 2

HCID 131596111-Chloro-1,1-difluoro-5,5-dimethyl-2,4-hexanedioneHCID 53630039Ethylorthoformate

생성물 1

HCID 540391191-Chloro-1,1-difluoro-5,5-dimethyl-3-ethoxymethylene-2,4-hexanedione수율 43.4%

시약·촉매·용매 1

HCID 7918Acetic Anhydride용매

실험 절차

12.4 g of 1-chloro-1,1-difluoro-5,5-dimethyl-2,4-hexanedione and 12.4 g of ethyl orthoformate were added to 50 ml of acetic anhydride, and the mixture was refluxed under heating for 2 hours. After the solvent was distilled off under reduced pressure, the residue was subjected to vacuum distillation to obtain 6.8 g of the desired product. (b.p. 105°-107° C./2 mmHg)

후처리

  1. temperaturethe mixture was refluxed
  2. temperatureunder heating for 2 hours
  3. distillationAfter the solvent was distilled off under reduced pressure
  4. distillationthe residue was subjected to vacuum distillation

출처 및 근거

ORD 기록
ord-370f8552418e4e5f8a4127795cea9c3d
출처 데이터셋
uspto-grants-1998_06
특허 번호
US05773388

반응 노트

불러오는 중…