18-Crown-6 → HCID 15452060, 화합물

HRID 1005487노트

반응식

HRID 1005487 반응식
Cl[C:2]1[C:9]([Cl:10])=[CH:8][CH:7]=[C:6]([C:11]([F:14])([F:13])[F:12])[C:3]=1[C:4]#[N:5].[F-:15].[K+].C1OCCOCCOCCOCCOCCOC1>CN(C)C=O>[Cl:10][C:9]1[C:2]([F:15])=[C:3]([C:6]([C:11]([F:14])([F:13])[F:12])=[CH:7][CH:8]=1)[C:4]#[N:5]

참가 물질

5

반응물 3

HCID 2855718-Crown-6HCID 522689Potassium FluorideHCID 109775462,3-Dichloro-6-(trifluoromethyl)benzonitrile

생성물 1

HCID 15452060HCID 15452060, 화합물수율 72.7%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
100 °C

실험 절차

To a solution of 0.96 g of 2,3-dichloro-6-trifluoromethylbenzonitrile in 7 ml of N,N-dimethylformamide was added 0.46 g of spray-dried potassium fluoride and 0.1 g of 18-crown-6-ether and the mixture was stirred for 6 hours at 100° C. under a nitrogen atmosphere. After cooling, the reaction mixture was poured into ice water and extracted with ethyl acetate. The organic layer was washed with saturated saline solution and dried over anhydrous magnesium sulfate. After distilling the solvent under reduced pressure, the crude product obtained was purified by using silica gel column chromatography to obtain 0.65 g of the title compound(mp. 43-44° C.).

후처리

  1. temperatureAfter cooling
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with saturated saline solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationAfter distilling the solvent under reduced pressure
  6. customthe crude product obtained
  7. customwas purified

출처 및 근거

ORD 기록
ord-9cbea0cc61ff4c699ec7bf5d529e5133
출처 데이터셋
uspto-grants-2000_04
특허 번호
US06054605

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