Sodium Hydroxide → 6-(Trifluoromethyl)pyrazin-2-amine

温度

20 °C

A mixture of 6.6 g. of 3,3-dibromo-1,1,1-trifluoropropanone, 60 ml. of water, and 6.6 g. sodium acetate was refluxed for about 10 minutes. The solution thus obtained was cooled and added dropwise to a solution of 6 g. of aminoacetamidine dihydrobromide in 90 ml. of methanol cooled to a temperature of about -30° C., followed by the addition of a solution of 3.6 g. of sodium hydroxide pellets in 25 ml. of water. The reaction mixture was stirred and warmed gradually to about 20° C. over a period of about two hours. The reaction product mixture was concentrated in vacuo to remove the methanol, and the residue extracted with ethyl acetate. There was obtained product weighing 3.6 g. and having a melting point of about 133°-136° C. after recrystallization from a mixture of benzene and hexane. The product was identified by NMR spectrum and elemental analyses as 2-amino-6-trifluoromethylpyrazine.

1. additionA mixture of 6.6 g
2. customThe solution thus obtained
3. temperaturewas cooled
4. additionadded dropwise to a solution of 6 g
5. additionfollowed by the addition of a solution of 3.6 g
6. concentrationThe reaction product mixture was concentrated in vacuo
7. customto remove the methanol
8. extractionthe residue extracted with ethyl acetate
9. customThere was obtained product
10. customafter recrystallization
11. additionfrom a mixture of benzene and hexane

ORDレコード

ord-bf746a89d6334d0fb45ee27a97f3e1e3

出典データセット

uspto-grants-1981_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04293552