Sodium Iodide → Rac-2-(methylamino)-1-pyrimidin-2-ylethanol
反応式
Cl[CH2:2][CH:3]([C:5]1[N:10]=[CH:9][CH:8]=[CH:7][N:6]=1)[OH:4].[I-].[Na+].[CH3:13][NH2:14]>CO>[CH3:13][NH:14][CH2:2][CH:3]([C:5]1[N:10]=[CH:9][CH:8]=[CH:7][N:6]=1)[OH:4]参加物
5
実験手順
In a pressure bottle was placed 2-chloro-1-pyrimidin-2-ylethanol (3.525 g, 22.24 mmol), sodium iodide (0.344 g, 2.29 mmol) and a 2M. methylamine solution (160 ml, 320 mmol) in methanol. The bottle was sealed and heated at 62° for 17 hr. The solvent was evaporated and the residue stirred with 10% MeOH—CHCl3. Filtration and evaporation gave a dark oil that was chromatographed over silica gel (90 g) eluting with 5-10% MeOH—CH2Cl2 containing 1% triethylamine The product was obtained as an amber oil (1.625 g).
後処理
- customThe bottle was sealed
- temperatureheated at 62° for 17 hr
- customThe solvent was evaporated
- filtrationFiltration and evaporation
- customgave a dark oil that
- customwas chromatographed over silica gel (90 g)
- washeluting with 5-10% MeOH—CH2Cl2 containing 1% triethylamine The product
出典と根拠
- ORDレコード
- ord-db4df481182b4e45adbff5ce1c0d179a
- 出典データセット
- uspto-grants-2005_02
- 特許番号
- US06852731B2
反応ノート
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