تفاعل #78385

معادلة التفاعل

methyl 2-[1-amino-1-(4-fluorophenyl)methylene]-4-methyl-3-oxopentanoate

toluene

N-cyano-N-methylmethanesulphonamide

→

crude product

المردود 80.3%

Methyl 4-(4-fluorophenyl)-6-isopropyl-2-(N-methanesulphonyl-N-methylamino)pyrimidine-5-carboxylate

المردود 80.3%

المذيبات

water

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةIt was then cooled to room temperature
2. 2
   أخرىThe organic phase was separated off
3. 3
   استخلاصthe aqueous phase was extracted with ethyl acetate (30 ml)
4. 4
   غسيلThe combined organic phases were washed with 30 ml of water
5. 5
   تجفيفdried over magnesium sulphate
6. 6
   ترشيحAfter filtering
7. 7
   تركيزconcentrating the solution in a water-jet vacuum
8. 8
   أخرىdrying in vacuo

الإجراء التجريبي

10.0 g (37.7 mmol) of methyl 2-[1-amino-1-(4-fluorophenyl)methylene]-4-methyl-3-oxopentanoate were introduced into 50 ml of toluene, together with 10.17 g (75.4 mmol) of N-cyano-N-methylmethanesulphonamide and the mixture was treated at room temperature with 3.61 g (18.9 mmol) of titanium tetrachloride. The reaction progressed exothermically. The red-orange-coloured suspension was heated to 110° C. and stirred for 4.5 h. It was then cooled to room temperature and treated with 30 ml of water. The organic phase was separated off and the aqueous phase was extracted with ethyl acetate (30 ml). The combined organic phases were washed with 30 ml of water and dried over magnesium sulphate. After filtering and concentrating the solution in a water-jet vacuum and drying in vacuo, 11.54 g of crude product were obtained in the form of a tacky oil.

المصدر