Water → HCID 86598208、化合物

HRID 2217255ノート

反応式

HRID 2217255 の反応式
[NH2:1][C:2]1[N:3]=[C:4]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[C:5]([C:14]2[CH:15]=[CH:16][C:17](=[O:23])[N:18]([CH:20]([CH3:22])[CH3:21])[CH:19]=2)=[N:6][C:7]=1[C:8]#[C:9][Si](C)(C)C.C([O-])([O-])=O.[K+].[K+].O.CCOC(C)=O>CO>[NH2:1][C:2]1[N:3]=[C:4]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[C:5]([C:14]2[CH:15]=[CH:16][C:17](=[O:23])[N:18]([CH:20]([CH3:22])[CH3:21])[CH:19]=2)=[N:6][C:7]=1[C:8]#[CH:9]

参加物

6

反応物 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 69103390HCID 69103390、化合物

生成物 1

HCID 86598208HCID 86598208、化合物収率 40.6%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
25 °C

実験手順

A mixture of 5-{5-amino-3-phenyl-6-[(trimethylsilyl)ethynyl]-2-pyrazinyl}-1-isopropyl-2(1H)-pyridone (300 mg) and sat. K2CO3 in MeOH (4.5 ml) was stirred at 25° C. for 3 hours. Water and EtOAc were poured into the mixture, and the organic layer was separated, washed with water and brine, and dried over MgSO4. The solvent was removed under reduced pressure. The residue was purified by short column (silica-gel; CH2Cl2) and recrystallized from EtOH to give 5-(5-amino-6-ethynyl-3-phenyl-2-pyrazinyl)-1-isopropyl-2(1H)-pyridone (100 mg).

後処理

  1. customthe organic layer was separated
  2. washwashed with water and brine
  3. dry with materialdried over MgSO4
  4. customThe solvent was removed under reduced pressure
  5. customThe residue was purified by short column (silica-gel; CH2Cl2)
  6. customrecrystallized from EtOH

出典と根拠

ORDレコード
ord-e7304bafd9dc40f08cabe2ff1347945f
出典データセット
uspto-grants-2008_08
特許番号
US07407961B2

反応ノート

読み込み中…