Water → HCID 86631565, 화합물

HRID 885816노트

반응식

HRID 885816 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:9](=[O:26])[CH2:10][C:11]([C:17]2[CH:22]=[C:21]([Br:23])[C:20]([F:24])=[C:19]([Br:25])[CH:18]=2)(O)[C:12]([F:15])([F:14])[F:13])[CH:5]=[CH:6][C:7]=1[CH3:8].S(Cl)(Cl)=O.N1C=CC=CC=1.O>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:3]=[C:4]([C:9](=[O:26])[CH:10]=[C:11]([C:17]2[CH:22]=[C:21]([Br:23])[C:20]([F:24])=[C:19]([Br:25])[CH:18]=2)[C:12]([F:15])([F:14])[F:13])[CH:5]=[CH:6][C:7]=1[CH3:8]

참가 물질

6

반응물 4

HCID 962WaterHCID 1049PyridineHCID 24386Thionyl ChlorideHCID 86631563HCID 86631563, 화합물

생성물 1

HCID 86631565HCID 86631565, 화합물수율 101.4%

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
5 °C

실험 절차

To a stirred solution of 1-(3-chloro-4-methylphenyl)-3-(3,5-dibromo-4-fluorophenyl)-4,4,4-trifluoro-3-hydroxy-butan-1-one (1.40 g) in toluene (3 mL) at 80° C. was added thionyl chloride (0.68 g) and pyridine (0.46 g). The mixture was stirred at same temperature for 2 hours. The resulting mixture was then cooled to 5° C. and water (3 mL) was added, and the mixture was allowed to stir and warm to ambient temperature. The layers were separated, and the organic phase was poured into 2N aqueous sodium hydroxide solution (3 mL). After stirring 0.5 hour at room temperature, the organic layer was separated, washed with brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to afford the crude title compound as a yellow oil (1.37 g), which was used in the next step without purification.

후처리

  1. stirringto stir
  2. temperaturewarm to ambient temperature
  3. customThe layers were separated
  4. additionthe organic phase was poured into 2N aqueous sodium hydroxide solution (3 mL)
  5. stirringAfter stirring 0.5 hour at room temperature
  6. customthe organic layer was separated
  7. washwashed with brine
  8. dry with materialdried over anhydrous magnesium sulfate
  9. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-da45876ac39442f6a303d4f3522a4d71
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08242283B2

반응 노트

불러오는 중…