Ethanamine, 2-(4-methylphenoxy)-, hydrochloride (1:1) → HCID 68677501、化合物

HRID 2233044ノート

反応式

HRID 2233044 の反応式
[C:1]([C:5]1[N:6]=[C:7](Cl)[C:8]2[N:9]([C:11](=[O:14])[NH:12][N:13]=2)[CH:10]=1)([CH3:4])([CH3:3])[CH3:2].Cl.[C:17]1([CH3:27])[CH:22]=[CH:21][C:20]([O:23][CH2:24][CH2:25][NH2:26])=[CH:19][CH:18]=1>CN(C=O)C>[C:1]([C:5]1[N:6]=[C:7]([NH:26][CH2:25][CH2:24][O:23][C:20]2[CH:21]=[CH:22][C:17]([CH3:27])=[CH:18][CH:19]=2)[C:8]2[N:9]([C:11](=[O:14])[NH:12][N:13]=2)[CH:10]=1)([CH3:4])([CH3:3])[CH3:2]

参加物

4

反応物 2

HCID 17233812Ethanamine, 2-(4-methylphenoxy)-, hydrochloride (1:1)HCID 68676527HCID 68676527、化合物

生成物 1

HCID 68677501HCID 68677501、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

To a solution of 60 mg of 6-tert-butyl-8-chloro-2H-[1,2,4]triazolo[4,3-a]pyrazin-3-one and 100 mg of 2-p-tolyloxy-ethylamine hydrochloride in DMF (2.0 mL) was added 60 mg of TEA. The mixture was heated to 80° C. for three h and then was cooled to ambient temperature and partitioned between EtOAc and water. The organic layer was washed with sat. sodium chloride solution and then dried over sodium sulfate, filtered, and concentrated. The residue was purified by silica gel chromatography to afford the title compound as a white solid. MS (M+H+)=342.5.

後処理

  1. temperaturewas cooled to ambient temperature
  2. custompartitioned between EtOAc and water
  3. washThe organic layer was washed with sat. sodium chloride solution
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe residue was purified by silica gel chromatography

出典と根拠

ORDレコード
ord-753eecbcf58146e0b9edfc086a5ad1ef
出典データセット
uspto-grants-2010_05
特許番号
US07709473B2

反応ノート

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