Potassium Carbonate → 1-(2-Hydroxy-3,3,3-trichloropropyl)-5-bromopyrimid-2-one

A stirred mixture of 5-bromopyrimid-2-one (0.009 mol), 1,2-epoxy-3,3,3-trichloropropane (0.009 mol) and K2CO3 (33 mg) in dimethylformamide (40 ml ) was heated at 80° C. for 4 h. The reaction mixture was then evaporated to dryness at reduced pressure (1 mm Hg). The crystalline residue was triturated with a little ether and dissolved in ethyl acetate. The filtered ethyl acetate solution was concentrated to about 50 ml and left in the cold when the product crystallized out in 52% yield. m.p. 210°-212° C. (ethyl acetate).

1. customThe reaction mixture was then evaporated to dryness at reduced pressure (1 mm Hg)
2. customThe crystalline residue was triturated with a little ether
3. dissolutiondissolved in ethyl acetate
4. concentrationThe filtered ethyl acetate solution was concentrated to about 50 ml
5. waitleft in the cold when the product
6. customcrystallized out in 52% yield

ORDレコード

ord-81e1ed89da8d4ea4881280598e77f346

出典データセット

uspto-grants-1983_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04395406