Tetrahydrofuran → HCID 14624364, 화합물

HRID 1650773

반응식

HRID 1650773 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([O:8][C:9]([F:12])([F:11])[F:10])[CH:5]=[C:4]([Cl:13])[C:3]=1[NH:14][N:15]=[C:16](Cl)[C:17]([CH3:20])([CH3:19])[CH3:18].[CH2:22]([N:24]([CH2:27][CH3:28])[C:25]#[N:26])[CH3:23].O1CCCC1.C(N(CC)CC)C>O>[Cl:1][C:2]1[CH:7]=[C:6]([O:8][C:9]([F:12])([F:11])[F:10])[CH:5]=[C:4]([Cl:13])[C:3]=1[N:14]1[C:25]([N:24]([CH2:27][CH3:28])[CH2:22][CH3:23])=[N:26][C:16]([C:17]([CH3:20])([CH3:19])[CH3:18])=[N:15]1

참가 물질

6

반응물 4

HCID 8028TetrahydrofuranHCID 8471TriethylamineHCID 12050DiethylcyanamideHCID 86743925HCID 86743925, 화합물

생성물 1

HCID 14624364HCID 14624364, 화합물수율 87.1%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

7.3 g (0.02 mol) of 2,2-dimethylpropionyl chloride 2,6-dichloro-4-trifluoromethoxyphenylhydrazone and 2.0 g (0.02 mol) of N,N-diethylcyanamide were added to 100 ml of tetrahydrofuran, and 2.2 g (0.02 mol) of triethylamine was dropwise added under reflux and stirring. After completion of the dropwise addition, the mixture was stirred at the same temperature for 0.5 hour. After cooling, the reaction solution was poured into water, and the precipitate was extracted with chloroform. The chloroform layer was washed with water and dried, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography to obtain 7.4 g (yield: 87.1%) of the desired compound as a pale yellow liquid. Refractive index nD20 : 1.4940.

후처리

  1. additionwas dropwise added
  2. temperatureunder reflux
  3. additionAfter completion of the dropwise addition
  4. stirringthe mixture was stirred at the same temperature for 0.5 hour
  5. temperatureAfter cooling
  6. extractionthe precipitate was extracted with chloroform
  7. washThe chloroform layer was washed with water
  8. customdried
  9. distillationthe solvent was distilled off under reduced pressure
  10. customThe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-eb05cccaa5ee4164ab241518e4b43c55
출처 데이터셋
uspto-grants-1990_05
특허 번호
US04925864

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