Triethylamine → 2-Bromo-1-(4-pyrimidin-2-ylpiperazin-1-yl)ethanone
反応式
[Br:1][CH2:2][C:3](Br)=[O:4].[N:6]1[CH:11]=[CH:10][CH:9]=[N:8][C:7]=1[N:12]1[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1.C(N(CC)CC)C>C1COCC1>[Br:1][CH2:2][C:3]([N:15]1[CH2:16][CH2:17][N:12]([C:7]2[N:6]=[CH:11][CH:10]=[CH:9][N:8]=2)[CH2:13][CH2:14]1)=[O:4]参加物
5
実験手順
20.2 g bromacetylbromide was dropped to 16.5 g 1-pyrimidin-2-yl-piperazin and 10.2 g triethylamine in 250 mL THF. The reaction was stirred over night at RT and evaporated. The residue was extracted with DCM and water. The organic layer was evaporated and the residue was crystallized with petrolether and then purified by chromatography on silica gel (DCM/MeOH:95/5) to yield 36 mg of the desired compound.
後処理
- customevaporated
- extractionThe residue was extracted with DCM and water
- customThe organic layer was evaporated
- customthe residue was crystallized with petrolether
- custompurified by chromatography on silica gel (DCM/MeOH:95/5)
出典と根拠
- ORDレコード
- ord-f971d6ac5dfa4b12a4f4c5f44ffe44c2
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08822464B2
反応ノート
読み込み中…