Water → HCID 19068959, 화합물

HRID 1735114노트

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HRID 1735114 반응식
[CH3:1][N:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4]2[CH:11]=[CH:12][S:13][C:3]1=2.[F:14][C:15]([F:26])([F:25])[C:16](OC1C=CC=CN=1)=[O:17].[Al+3].[Cl-].[Cl-].[Cl-].O>ClCCCl>[CH3:1][N:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4]2[C:11]([C:16](=[O:17])[C:15]([F:26])([F:25])[F:14])=[CH:12][S:13][C:3]1=2

참가 물질

6

반응물 4

HCID 962WaterHCID 46382142-(Trifluoroacetoxy)pyridineHCID 6451240Aluminum(III) ChlorideHCID 19068992HCID 19068992, 화합물

생성물 1

HCID 19068959HCID 19068959, 화합물

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

반응 조건

온도
-10 °C

실험 절차

A mixture of 1 g of (73) and 1.1 g of 2-trifluoromethylcarbonyloxypyridine, prepared according to the literature (Keumi, T. et. al. Chem. Lett. 5 (1990) 783-6), in 25 ml of 1,2-dichloroethane, was cooled to -10° C. with stirring. 1.5 g of AlCl3 was added over 15 minutes at this temperature, the reaction mixture was stirred at 0° C. for 4 hours, and at room temperature overnight. Water was added, the phases separated, and the organic phase dried and evaporated to dryness. Purification by column chromatography on silica gel in toluene gave the pure (74). Yield 590 mg. M.p. 138°-40° C.

후처리

  1. customprepared
  2. stirringthe reaction mixture was stirred at 0° C. for 4 hours
  3. customat room temperature
  4. customovernight
  5. customthe phases separated
  6. customthe organic phase dried
  7. customevaporated to dryness
  8. customPurification by column chromatography on silica gel in toluene

출처 및 근거

ORD 기록
ord-0a2765c1086248439f7cef9063d18399
출처 데이터셋
uspto-grants-1996_07
특허 번호
US05536721

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