Methyl iodide → (7-(Methylthio)[1,3]thiazolo[5,4-d]pyrimidin-2-yl)methanol
反応式
[SH:1][C:2]1[C:3]2[N:10]=[C:9]([CH2:11][OH:12])[S:8][C:4]=2[N:5]=[CH:6][N:7]=1.I[CH3:14]>[OH-].[Na+]>[CH3:14][S:1][C:2]1[C:3]2[N:10]=[C:9]([CH2:11][OH:12])[S:8][C:4]=2[N:5]=[CH:6][N:7]=1参加物
4
実験手順
A solution of (7-mercapto[1,3]thiazolo[5,4-d]pyrimidin-2-yl)methanol (Intermediate 75) (48.3 g) and iodomethane (16.6 mL) in 2M NaOH (450 mL) was stirred at ambient temperature for 5 hours. The crude product was collected by filtration, suspended in water and acidified by addition of 2N HCl. The flocculant solid was collected by filtration, washed with water (200 mL) and ether (200 mL) and dried under vacuum over phosphorus pentoxide to give the title compound as a pale brown solid (27.5 g, 53%);
後処理
- filtrationThe crude product was collected by filtration
- additionacidified by addition of 2N HCl
- filtrationThe flocculant solid was collected by filtration
- washwashed with water (200 mL) and ether (200 mL)
- dry with materialdried under vacuum over phosphorus pentoxide
出典と根拠
- ORDレコード
- ord-03887c52836241e78ca4ac93d53adbe9
- 出典データセット
- uspto-grants-2008_09
- 特許番号
- US07427616B2
反応ノート
読み込み中…