Potassium Carbonate → Dimethyl (2,2,2-trichloroethylidene)propanedioate

In a 0.3-liter four-necked flask, 7.06 g (41.6 mmol) of 2-amino-6-chloropurine (manufactured by Sumika Fine Chemicals Co., Ltd.) and 12.4 g (89.7 mmol) of potassium carbonate were added to 188 ml of N,N-dimethylformamide, and the resulting mixture was stirred at room temperature for 30 minutes. Next, 16.0 g (61.2 mmol) of dimethyl 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 four hours 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 12.14 g (34.7 mmol) of white crystals of 2-amino-6-chloro-9-(3,3-dicarbomethoxy-2,2-dichlorocyclopropyl)purine. The yield was 83.4%.

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

ORD record

ord-1afe536f8fa94abe8f5b7d164f50dc6d

Source dataset

uspto-grants-2002_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06342603B1