Hexahydro-1,4-diazepine → 1-pyrimidin-2-yl-1,4-diazepane
反応式
[NH:1]1[CH2:7][CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.Cl[C:9]1[N:14]=[CH:13][CH:12]=[CH:11][N:10]=1>C(O)C>[N:10]1[CH:11]=[CH:12][CH:13]=[N:14][C:9]=1[N:1]1[CH2:7][CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1参加物
4
実験手順
To a solution of homopiperazine (3.5 g, 35 mmol) in ethanol (100 ml) at 40° C., was added portionwise 2-chloropyrimidine (2.0 g, 17.5 mmol). The mixture was stirred for 1 hour then concentrated in vacuo. The residue was dissolved in methylene chloride (75 ml) and washed with a saturated solution of sodium bicarbonate and brine. Layers were separated, and the organic layer was dried over magnesium sulfate and concentrated. The resulting residue was purified by flash chromatography and a semi-solid (1.0 g) was collected and used as is.
後処理
- concentrationthen concentrated in vacuo
- dissolutionThe residue was dissolved in methylene chloride (75 ml)
- washwashed with a saturated solution of sodium bicarbonate and brine
- customLayers were separated
- dry with materialthe organic layer was dried over magnesium sulfate
- concentrationconcentrated
- customThe resulting residue was purified by flash chromatography
- customa semi-solid (1.0 g) was collected
出典と根拠
- ORDレコード
- ord-28d31164e63f4d848ec51404d881586d
- 出典データセット
- uspto-grants-2014_07
- 特許番号
- US08772291B2
反応ノート
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