反応式
[SH:1][C:2]1[N:7]=[C:6]([OH:8])[CH:5]=[C:4]([OH:9])[N:3]=1.[OH-].[Na+].CN1C[CH2:16][C:15](=O)[CH2:14]1.ICCC.Cl>O>[CH2:14]([S:1][C:2]1[N:7]=[C:6]([OH:8])[CH:5]=[C:4]([OH:9])[N:3]=1)[CH2:15][CH3:16]参加物
7
実験手順
A solution of 2-mercaptopyrimidine-4,6-diol (25 g, 173.61 mmol, 1.00 equiv.), sodium hydroxide (15.8 g, 395.00 mmol, 2.27 equiv.), 1-methylpyrrolidin-3-one (50 mL), and 1-iodopropane (30.6 g, 180.00 mmol, 1.05 equiv.) dissolved in water (60 mL) was stirred at ambient temperature for about 48 hours. The pH value of the solution was adjusted to 2-3 by adding hydrochloric acid. The solids were then collected by filtration to give the product as an off-white solid (35 g; (crude)). 1H NMR (300 MHz, DMSO-d6) δ: 11.78 (b, 1H), 10.30 (b, 1H), 5.13 (s, 1H), 3.07 (t, J=7.2 Hz, 2H), 1.58-1.70 (m, 2H), 0.96 (t, J=7.2 Hz, 2H).
後処理
- filtrationThe solids were then collected by filtration
出典と根拠
- ORDレコード
- ord-0fcc2bd8f35f432c94050e3b3773ac1c
- 出典データセット
- uspto-grants-2014_08
- 特許番号
- US08802850B2
関連ノート
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