Methanesulfonic Acid → 2-Mercapto-3-methyl-6-(pyrimidin-4-YL)-3H-pyrimidin-4-one
反応式
O=[C:2]([C:9]1[CH:14]=[CH:13][N:12]=[CH:11][N:10]=1)[CH2:3][C:4]([O:6]CC)=O.[CH3:15][NH:16][C:17]([NH2:19])=[S:18].C1CCN2C(=NCCC2)CC1.CS(O)(=O)=O>C(O)C.O>[SH:18][C:17]1[N:16]([CH3:15])[C:4](=[O:6])[CH:3]=[C:2]([C:9]2[CH:14]=[CH:13][N:12]=[CH:11][N:10]=2)[N:19]=1参加物
7
実験手順
A solution of ethyl 3-oxo-3-(4-pyrimidyl)propionate (34.1 g, 176 mmol), N-methyl thiourea (47.5 g, 527 mmol) and 1,8-diazabicyclo[5,4,0]-7-undecene (26.3 ml, 176 mmol) in ethanol (340 ml) was refluxed for 2 hours and the solution of methanesulfonic acid (16.9 g, 176 mmol) in water (70 ml) was added after cooling by ice-water. The precipitate was washed with water, filtered and dried to give the title compound (30.2 g, 78%).
後処理
- washThe precipitate was washed with water
- filtrationfiltered
- customdried
出典と根拠
- ORDレコード
- ord-ac8eeacccb1d48179905b62cb47d5d59
- 出典データセット
- uspto-grants-2015_08
- 特許番号
- US09108957B2
反応ノート
読み込み中…