Thiomorpholine → HCID 5185429、化合物
反応式
[NH2:1][C:2]1[N:7]([OH:8])[C:6](=[NH:9])[N:5]=[C:4](Cl)[CH:3]=1.[NH:11]1[CH2:16][CH2:15][S:14][CH2:13][CH2:12]1>CN(C)C=O>[NH2:1][C:2]1[N:7]([OH:8])[C:6](=[NH:9])[N:5]=[C:4]([N:11]2[CH2:16][CH2:15][S:14][CH2:13][CH2:12]2)[CH:3]=1参加物
4
反応条件
- 温度
- 110 °C
実験手順
A mixture of 16.1 g of 6-amino-4-chloro-1,2-dihydro-2-imino-1-pyrimidinol, 32.1 g of thiomorphline, and 75 ml of dimethyl formamide is heated at 110°C in a nitrogen atmosphere for 17 hours. The solvent is removed under high vacuum. The residue is dissolved in 2 normal hydrochloric acid, and the resulting solution made basic with 5% ammonium hydroxide. There is deposited 13.0 g (57%) of a crystalline solid mp 242°(dec). Recrystallization from methanol-ethanol gives an off-white crystalline solid, mp 246°C(dec).
後処理
- customThe solvent is removed under high vacuum
- dissolutionThe residue is dissolved in 2 normal hydrochloric acid
- customRecrystallization from methanol-ethanol
- customgives an off-white crystalline solid, mp 246°C(dec)
出典と根拠
- ORDレコード
- ord-5971cbac111a4e01b2a733085311e34e
- 出典データセット
- uspto-grants-1976_08
- 特許番号
- US03973016
反応ノート
読み込み中…