Acetic Acid → HCID 9817216, 화합물

HRID 968076

반응식

HRID 968076 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](N(C)C)=[CH:9][C:10]2[CH:15]=[CH:14][C:13]([C:16]([F:19])([F:18])[F:17])=[CH:12][CH:11]=2)=[CH:4][CH:3]=1.C(O)(=[O:25])C.Cl>O>[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:25])[CH2:9][C:10]2[CH:15]=[CH:14][C:13]([C:16]([F:19])([F:18])[F:17])=[CH:12][CH:11]=2)=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 697465101-(4-fluorophenyl)-2-(4-trifluoromethylphenyl)-N,N-dimethylethenylamine

생성물 1

HCID 9817216HCID 9817216, 화합물수율 90.3%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Into a 200 ml four-necked flask equipped with a thermometer, a stirrer and a reflux condenser, 15.5 g (50 mmol) of 1-(4-fluorophenyl)-2-(4-trifluoromethylphenyl)-N,N-dimethylethenylamine, 80 ml of acetic acid and 30 ml of concentrated hydrochloric acid were charged and reacted with stirring for two hours under refluxing under heating by an oil bath. After completion of reaction, 500 ml of water was added, and precipitated crystals were collected by filtration and washed with a 2% sodium hydrogen carbonate aqueous solution and water. Then, the crystals were further washed and purified with 20 ml of n-hexane and then vacuum-dried to obtain 12.7 g (yield: 90.3%) of the desired compound (melting point: 93-95° C.) as slightly yellow crystals.

후처리

  1. additionwere charged
  2. customreacted
  3. temperatureunder refluxing
  4. temperatureunder heating by an oil bath
  5. additionwas added
  6. customprecipitated crystals
  7. filtrationwere collected by filtration
  8. washwashed with a 2% sodium hydrogen carbonate aqueous solution and water
  9. washThen, the crystals were further washed
  10. custompurified with 20 ml of n-hexane
  11. customvacuum-dried

출처 및 근거

ORD 기록
ord-d32059cc5c3346b889444bdb232ea8aa
출처 데이터셋
uspto-grants-2005_10
특허 번호
US06956132B2

연결된 노트

불러오는 중…