反应 #6977

ord-55368fddc085434994f442da384179d4

反应条件

温度
40°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他the volatiles were removed in vacuo
  2. 2
    其他the solid formed
  3. 3
    过滤was collected by filtration
  4. 4
    洗涤rinsed with water
  5. 5
    其他dried

实验过程

A mixture of ethyl-6-amino-nicotinate (2.5 g, 15 mmol) and benzoyl isothiocyanate (2.45 g, 15 mmol) in THF (20 mL) was heated at 40° C. for 4 h. To this mixture at RT, was added sodium ethoxide (2.04 g, 30 mmol) in ethanol (10 mL). After stirring the resulting mixture at RT for 16 h, the volatiles were removed in vacuo. The residue was suspended in aqueous NH4Cl and the solid formed was collected by filtration, rinsed with water and dried to afford 6-thioureido-nicotinic acid ethyl ester as a white solid (2.6 g, 77% yield). LC/MS; (M+H)+=226.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07084160B2uspto-grants-2006_08