Water → HCID 68535315, 화합물

HRID 1993684노트

반응식

HRID 1993684 반응식
[C:1]1([CH3:17])[CH:6]=[CH:5][C:4]([N:7]2[C:11]([NH2:12])=[CH:10][C:9]([Si:13]([CH3:16])([CH3:15])[CH3:14])=[N:8]2)=[CH:3][CH:2]=1.C(=O)([O-])[O-].[K+].[K+].O.Cl[C:26]([O:28][CH2:29][C:30]([Cl:33])([Cl:32])[Cl:31])=[O:27]>C(OCC)(=O)C>[Cl:31][C:30]([Cl:33])([Cl:32])[CH2:29][O:28][C:26](=[O:27])[NH:12][C:11]1[N:7]([C:4]2[CH:3]=[CH:2][C:1]([CH3:17])=[CH:6][CH:5]=2)[N:8]=[C:9]([Si:13]([CH3:16])([CH3:15])[CH3:14])[CH:10]=1

참가 물질

6

반응물 4

HCID 962Water2회HCID 11430Potassium CarbonateHCID 870632,2,2-Trichloroethyl chloroformateHCID 68540206HCID 68540206, 화합물

생성물 1

HCID 68535315HCID 68535315, 화합물수율 96%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

Place 2-p-tolyl-5-trimethylsilanyl-2H-pyrazol-3-ylamine (170 mg, 0.693 mmol) in ethyl acetate (10 mL). Add potassium carbonate (191 mg, 1.38 mmol) and water (2 mL). Stir the reaction and add trichloroethyl chloroformate (0.114 mL, 0.831 mmol). Stir at room temperature for 18 hours. Add water and ethyl acetate. Separate organic layer and wash with saturated aq. sodium chloride. Collect organic layer, dry over Mg2SO4, filter, and concentrate under reduced pressure. Subject residue to silica gel chromatography eluting with 0-30% EtOAc:hexane to yield 280 mg (96%) of the title compound. MS(ES+): m/z=420.2 [M+H].

후처리

  1. customthe reaction
  2. stirringStir at room temperature for 18 hours
  3. washSeparate organic layer and wash with saturated aq. sodium chloride
  4. dry with materialCollect organic layer, dry over Mg2SO4
  5. filtrationfilter
  6. concentrationconcentrate under reduced pressure
  7. washSubject residue to silica gel chromatography eluting with 0-30% EtOAc

출처 및 근거

ORD 기록
ord-37e275c0e8a94250bb4b2f15aae55ccc
출처 데이터셋
uspto-grants-2010_01
특허 번호
US07652015B2

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