1,3-Dichloroacetone → HCID 178511217、化合物

温度

10 °C

Into a 500 mL round bottom flask equipped with an overhead stirrer and under an inert atmosphere was added 25 g of 1,3-dichloroacetone (0.197 mol) and 75 g of acetone. The reaction mixture was cooled to 10° C. and 23.2 g 2-imino-4-thiobiuret (0.197 mol) was added. The reaction mixture was stirred for one hour at 10 C. The reaction mixture was then heated to 40° C. and 15 g of thiourea (0.197 mol) was added, followed by the addition of 100 g of water. The mixture was heated to and held at 52° C. for one hour. Acetone was then removed by vacuum distillation. To the reaction mixture was added 100 g of water, 17 g of 3-chloropropionitrile (0.190 mol) and 40 g of isopropyl alcohol. The reaction mixture was cooled below 10° C. and 25 g of an aqueous solution of sodium hydroxide (80 g water) was added dropwise maintaining the reaction temperature below 10° C. The reaction mixture was for 2 hours, filtered and washed to produce 28 g of N-[4-(cyanoethylthiomethyl)-2-thiazolyl]guanidine product.

1. customInto a 500 mL round bottom flask equipped with an overhead stirrer and under an inert atmosphere
2. temperatureThe reaction mixture was then heated to 40° C.
3. temperatureThe mixture was heated to and
4. waitheld at 52° C. for one hour
5. customAcetone was then removed by vacuum distillation
6. temperatureThe reaction mixture was cooled below 10° C.
7. temperaturemaintaining the reaction temperature below 10° C
8. waitThe reaction mixture was for 2 hours
9. filtrationfiltered
10. washwashed

ORDレコード

ord-f3466171283b4e8baa7b035687e671be

出典データセット

uspto-grants-1999_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05856500