Trifluoroacetic acid → HCID 18369481, 화합물

HRID 1699801노트

반응식

HRID 1699801 반응식
FC(F)(F)C(O)=O.C([SiH](CC)CC)C.[CH3:15][C:16]1[CH:29]=[C:19]2[CH:20]=[C:21]([C:24]([O:26][CH2:27][CH3:28])=[O:25])[CH:22]=[CH:23][N:18]2[N:17]=1.[Cl:30][C:31]1[CH:38]=[C:37]([Cl:39])[CH:36]=[CH:35][C:32]=1[CH:33]=O>ClCCl>[Cl:30][C:31]1[CH:38]=[C:37]([Cl:39])[CH:36]=[CH:35][C:32]=1[CH2:33][C:29]1[C:16]([CH3:15])=[N:17][N:18]2[CH:23]=[CH:22][C:21]([C:24]([O:26][CH2:27][CH3:28])=[O:25])=[CH:20][C:19]=12

참가 물질

6

반응물 4

HCID 6422Trifluoroacetic acidHCID 12052TriethylsilaneHCID 134042,4-Dichlorobenzaldehyde2회HCID 22388192HCID 22388192, 화합물

생성물 1

HCID 18369481HCID 18369481, 화합물수율 65.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of trifluoroacetic acid (558 mg) and triethylsilane (1.14 g) in dry dichloromethane (2.0 ml) were added ethyl 2-methylpyrazolo[1,5-a]pyridine-5-carboxylate (200 mg) and 2,4-dichlorobenzaldehyde (189 mg), and the mixture was stirred at room temperature for 3 days. To the reaction mixture was added 2,4-dichlorobenzaldehyde (189 mg) and the mixture was stirred at room temperature for one day. This step was repeated three times. The reaction mixture was diluted with dichloromethane and washed with a saturated aqueous sodium hydrogencarbonate solution. The aqueous layer was extracted with dichloromethane. The organic layers were combined, dried over magnesium sulfate, and concentrated to dryness under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=9:1) and washed with isopropyl ether to give the objective compound (233 mg) as a white powder.

후처리

  1. stirringthe mixture was stirred at room temperature for one day
  2. washwashed with a saturated aqueous sodium hydrogencarbonate solution
  3. extractionThe aqueous layer was extracted with dichloromethane
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated to dryness under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=9:1)
  7. washwashed with isopropyl ether

출처 및 근거

ORD 기록
ord-10b83fe2f4b24c7ab49ef0b7cd22fb10
출처 데이터셋
uspto-grants-2002_02
특허 번호
US06348474B1

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