反应详情

A mixture of (4-methoxy-phenyl)-thiourea (3.0 g, 16.5 mmol) and a 45% aqueous solution of chloroacetaldehyde (12 mL, 82.4 mmol, 5.0 equiv) in EtOH (23 mL) is heated to reflux for 1 h. The resulting dark orange solution is allowed to cool to RT and concentrated in vacuo. NaHCO3 is then added to the oily residue until CO2 evolution subsides and a beige precipitate forms. The product is collected by vacuum filtration, washed thoroughly with water (600 mL), and dried in vacuo. Title compound: ES-MS: 207.0 [M+H]+; single peak at tR=5.32 min (System 1); Rf=0.17 (CH2Cl2/MeOH, 95/5).

1. temperatureto reflux for 1 h
2. concentrationconcentrated in vacuo
3. additionNaHCO3 is then added to the oily residue until CO2 evolution subsides
4. filtrationThe product is collected by vacuum filtration
5. washwashed thoroughly with water (600 mL)
6. customdried in vacuo