Acetone → HCID 66628195, 화합물

HRID 386533

반응식

HRID 386533 반응식
[OH-:1].[Na+].[Br:3][C:4]1[C:5]([CH3:10])=[N:6][NH:7][C:8]=1[CH3:9].Cl[C:12](Cl)(Cl)[C:13](O)([CH3:15])[CH3:14].CC(C)=[O:21]>>[Br:3][C:4]1[C:5]([CH3:10])=[N:6][N:7]([C:13]([CH3:15])([CH3:14])[C:12]([OH:21])=[O:1])[C:8]=1[CH3:9]

참가 물질

5

반응물 4

HCID 180AcetoneHCID 5977ChlorobutanolHCID 14798Sodium HydroxideHCID 769374-bromo-3,5-dimethyl-1H-pyrazole

생성물 1

HCID 66628195HCID 66628195, 화합물

실험 절차

To a cold (0° C.), well stirred suspension of NaOH (1.6 g, 40 mmoles) and 4-bromo-3,5-dimethylpyrazole (1.75 g, 10 mmoles) in acetone (100 mL), was added 2-(trichloromethyl)-propan-2-ol (3.54 g, 20 mmoles) portion-wise over 1 hour. The mixture was allowed to warm to room temperature overnight. The solvent was evaporated under reduced pressure. The residue was dissolved in water (100 mL) and washed with ether (50 mL). The aqueous phase was separated and acidified with conc. HCl to pH=3. The mixture was extracted with CH2Cl2 (3×50 mL) and the combined organics dried over Na2SO4. A colorless oil was obtained after the removal of the solvent under reduced pressure. MS(DCI+) m/z 263 (M+H)+.

후처리

  1. customThe solvent was evaporated under reduced pressure
  2. dissolutionThe residue was dissolved in water (100 mL)
  3. washwashed with ether (50 mL)
  4. customThe aqueous phase was separated
  5. extractionThe mixture was extracted with CH2Cl2 (3×50 mL)
  6. dry with materialthe combined organics dried over Na2SO4
  7. customA colorless oil was obtained
  8. customafter the removal of the solvent under reduced pressure

출처 및 근거

ORD 기록
ord-4947e44d8de84158927b1560771772bc
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08372841B2

연결된 노트

불러오는 중…