Sodium Hydroxide → HCID 45926015、化合物

HRID 1667853ノート

反応式

HRID 1667853 の反応式
[C:1]([C:5]1[CH:9]=[C:8]([NH2:10])[N:7]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[N:6]=1)([CH3:4])([CH3:3])[CH3:2].[OH-].[Na+].[C:19](Cl)(=[O:26])[O:20][CH2:21][C:22]([Cl:25])([Cl:24])[Cl:23]>C(OCC)(=O)C>[C:1]([C:5]1[CH:9]=[C:8]([NH:10][C:19](=[O:26])[O:20][CH2:21][C:22]([Cl:25])([Cl:24])[Cl:23])[N:7]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[N:6]=1)([CH3:4])([CH3:2])[CH3:3]

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 870632,2,2-Trichloroethyl chloroformateHCID 7706343-tert-butyl-1-phenyl-1H-pyrazol-5-amine

生成物 1

HCID 45926015HCID 45926015、化合物収率 55.6%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

To a two-phase solution of 3-tert-butyl-1-phenyl-1H-pyrazol-5-amine (5.0 g, 23 mmol) in ethyl acetate (45 mL)/3N aqueous sodium hydroxide (20 mL) was added 2,2,2-trichloroethyl chlorocarbonate (4.5 mL, 33 mmol) under ice-cooling, and the mixture was stirred at room temperature for 2 hr. The obtained organic layer was washed with 5% aqueous sodium hydrogencarbonate, water and saturated brine, dried over anhydrous sodium sulfate, and filtrated. The solvent was evaporated under reduced pressure to give the title compound (5.0 g, 55%) as a white powder.

後処理

  1. temperaturecooling
  2. washThe obtained organic layer was washed with 5% aqueous sodium hydrogencarbonate, water and saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. filtrationfiltrated
  5. customThe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-fc00cb38c42e4aca8c5f7d80fdf2c5b2
出典データセット
uspto-grants-2011_10
特許番号
US08044049B2

反応ノート

読み込み中…