Dimethylformamide → HCID 69522213, 화합물

HRID 856621노트

반응식

HRID 856621 반응식
[SH:1][C:2]1[CH:8]=[CH:7][C:5]([NH2:6])=[CH:4][C:3]=1[C:9]([F:12])([F:11])[F:10].Cl.Cl[CH2:15][C:16]1[N:20]([CH2:21][CH2:22][CH3:23])[CH:19]=[N:18][N:17]=1.C(=O)([O-])[O-].[K+].[K+].CN(C)C=O>O>[CH2:21]([N:20]1[CH:19]=[N:18][N:17]=[C:16]1[CH2:15][S:1][C:2]1[CH:8]=[CH:7][C:5]([NH2:6])=[CH:4][C:3]=1[C:9]([F:10])([F:11])[F:12])[CH2:22][CH3:23]

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 3048824HCID 3048824, 화합물HCID 229387553-chloromethyl-4-propyl-4H-1,2,4-triazole hydrochloride

생성물 1

HCID 69522213HCID 69522213, 화합물수율 85.5%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

4-mercapto-3-trifluoromethylaniline (1.0 g), 3-chloromethyl-4-propyl-4H-1,2,4-triazole hydrochloride (1.1 g) and potassium carbonate (1.4 g) were added to N,N-dimethylformamide (35 ml), and the mixture was stirred overnight at room temperature. The mixture was poured into water, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated brine, dried over anhydrous magnesium sulfate, and then, the solvent was evaporated. The residue was purified by silica gel column chromatography (elution solvent: triethylamine/methanol/ethyl acetate) to give 4-[(4-propyl-4H-1,2,4-triazol-3-yl)methylthio]-3-trifluoromethylaniline (1.4 g) as pale brown oil.

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with water and saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customthe solvent was evaporated
  5. customThe residue was purified by silica gel column chromatography (elution solvent: triethylamine/methanol/ethyl acetate)

출처 및 근거

ORD 기록
ord-fcc731197d274e719eb0d27844ad463a
출처 데이터셋
uspto-grants-2007_08
특허 번호
US07262185B2

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