Water → HCID 68535315、化合物

HRID 1993684ノート

反応式

HRID 1993684 の反応式
[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

参加物

6

反応物 4

HCID 962Water2 回HCID 11430Potassium CarbonateHCID 870632,2,2-Trichloroethyl chloroformateHCID 68540206HCID 68540206、化合物

生成物 1

HCID 68535315HCID 68535315、化合物収率 96%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

実験手順

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].

後処理

  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

出典と根拠

ORDレコード
ord-37e275c0e8a94250bb4b2f15aae55ccc
出典データセット
uspto-grants-2010_01
特許番号
US07652015B2

反応ノート

読み込み中…