Hydrochloric Acid → HCID 178477340、化合物

To a solution of ethyl propionate (1.2 mL, 10 mmol) in DMF (1 mL) was added sodium methoxide (740 mg, 13 mmol), and to this was added ethyl formate (560 μL, 6.7 mmol) very slowly over 1 h period. The reaction mixture was stirred for 30 min then 2-ethyl-2-thiopseudourea (1.3 g, 6.7 mmol) in methanol (2.5 mL) was added at once. The mixture was heated and maintained at reflux for 2 h, cooled to room temperature and acidified to pH 6 with concentrated HCl. The resulting slurry was kept in ice bath for 30 minutes. The solid was collected and was rinsed with methanol. The solid was dried under vacuum to give 154 mg of the title compound. Mass spectrum 171.1 (CI, M+1).

1. temperatureThe mixture was heated
2. temperaturemaintained
3. temperatureat reflux for 2 h
4. customfor 30 minutes
5. customThe solid was collected
6. washwas rinsed with methanol
7. customThe solid was dried under vacuum

ORDレコード

ord-c01007e9015e4fbebc490d43cfe309be

出典データセット

uspto-grants-2002_12

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06498165B1