Water → diethyl 2,2,2-trichloroethylidenemalonate

In a one-liter four-necked flask, 50.0 g (294.9 mmol) of 2-amino-6-chloropurine (manufactured by Sumika Fine Chemicals Co., Ltd.) and 88.2 g (648.0 mmol) of potassium carbonate were added to 650 ml of dimethylsulfoxide, and 26.1 g (1449.9 mmol) of water was then added to the resulting mixture. The resulting mixture was stirred at room temperature. Next, 127.4 g (440.0 mmol) of diethyl 2,2,2-trichloroethylidenemalonate, which was prepared by the process described in U.S. Pat. No. 3,495,012, was added to the resulting mixture, and the mixture was stirred for two hours and a half at room temperature. Thereafter, the reaction mixture was filtered, and the filtrate was poured into water. The precipitated crystals were collected by filtration, washed with 100 ml of water, and then dried under reduced pressure, to give 101.5 g (240.1 mmol) of white crystals of 2-amino-6-chloro-9-(3,3-dicarboethoxy-2,2-dichlorocyclopropyl)purine. The yield was 82.8%.

1. additionwas then added to the resulting mixture
2. addition3,495,012, was added to the resulting mixture
3. stirringthe mixture was stirred for two hours
4. customat room temperature
5. filtrationThereafter, the reaction mixture was filtered
6. additionthe filtrate was poured into water
7. filtrationThe precipitated crystals were collected by filtration
8. washwashed with 100 ml of water
9. customdried under reduced pressure

ORD record

ord-b0fd2021aa6b449c9827c86562a65764

Source dataset

uspto-grants-2000_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06156892