Ethyl 3-amino-4,4,4-trifluorocrotonate → 3-(4-chloro-5-ethylsulfonylamino-2-fluorophenyl)-6-trifluoromethyl-2,4(1H,3H)-pyrimidinedione

온도

5 °C

1.06 g (5.77 mmol) of ethyl 3-amino-4,4,4-trifluorocrotonate was dissolved in 6.2 ml of N,N-dimethylformamide and 0.82 g (14.4 mmol) of sodium methoxide was added thereto. The reaction mixture was cooled to not higher than 5° C. after 10 minutes, and 1.56 g (4.81 mmol) of ethyl 4-chloro-5-ethylsulfonylamino-2-fluorocarbanilate was added thereto. The resultant mixture was heated to 110° C. and reacted for 4 hours. After the reaction was completed, N,N-dimethylformamide was distilled off and the resultant product was dissolved in water. The thus-obtained solution was washed with diethyl ether 3 times and thereafter concentrated hydrochloric acid was added thereto to pH 2. The precipitated crystals were filtered out, washed with water and dried to obtain 1.54 g of the objective product (yield: 77%) in the form of light yellow crystals.

1. customreacted for 4 hours
2. distillationN,N-dimethylformamide was distilled off
3. dissolutionthe resultant product was dissolved in water
4. washThe thus-obtained solution was washed with diethyl ether 3 times
5. additionconcentrated hydrochloric acid was added
6. filtrationThe precipitated crystals were filtered out
7. washwashed with water
8. customdried

ORD 기록

ord-dbd92c8c458a4f7abe5413cf41b0ee55

출처 데이터셋

uspto-grants-1995_05

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US05416236