Potassium Carbonate → 1-[(Trimethylsilyl)methyl]-4-chloro-3-(2-nitro-3-chlorophenyl)pyrazole

HRID 259703

반응식

HRID 259703 반응식
C(=O)([O-])[O-].[K+].[K+].[Cl:7][C:8]1[C:9]([C:13]2[CH:18]=[CH:17][CH:16]=[C:15]([Cl:19])[C:14]=2[N+:20]([O-:22])=[O:21])=[N:10][NH:11][CH:12]=1.[CH3:23][Si:24]([CH2:27]Cl)([CH3:26])[CH3:25]>CN(C)C=O.CCCCCCC.C(OCC)(=O)C>[CH3:23][Si:24]([CH2:27][N:11]1[CH:12]=[C:8]([Cl:7])[C:9]([C:13]2[CH:18]=[CH:17][CH:16]=[C:15]([Cl:19])[C:14]=2[N+:20]([O-:22])=[O:21])=[N:10]1)([CH3:26])[CH3:25]

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 75361Silane, (chloromethyl)trimethyl-HCID 178526739HCID 178526739, 화합물

생성물 1

HCID 229164881-[(Trimethylsilyl)methyl]-4-chloro-3-(2-nitro-3-chlorophenyl)pyrazole

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 21899848Ethylacetate heptane용매

실험 절차

0.85 g of anhydrous potassium carbonate is added to a solution of 1.30 g of 4-chloro-3-(2-nitro-3-chlorophenyl)pyrazole and 0.70 g of (trimethylsilyl)methyl chloride in 30 ml of N,N-dimethylformamide. The reaction mixture is stirred for 12 hours at room temperature and diluted with 100 ml of an ether/H2O (1/1) mixture. The ether phase is dried over MgSO4, and concentrated under reduced pressure. The residual oil is purified by liquid chromatography on a silica column (eluent: heptane/ethyl acetate [50/50]).

후처리

  1. dry with materialThe ether phase is dried over MgSO4
  2. concentrationconcentrated under reduced pressure
  3. customThe residual oil is purified by liquid chromatography on a silica column (eluent: heptane/ethyl acetate [50/50])

출처 및 근거

ORD 기록
ord-dfb774097ecc471691ac23936fe250fe
출처 데이터셋
uspto-grants-1996_06
특허 번호
US05523280

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