تفاعل #657272

معادلة التفاعل

N-hydroxysuccinimide

dicyclohexylcarbodiimide

(Pyrimidin-2-ylsulfanyl)-acetic acid

→

(Pyrimidin-2-ylsulfanyl)-acetic acid-(2,5-dioxo-pyrrolidine-1-yl)-ester

المذيبات

DMF

ظروف التفاعل

المعالجة

1. 1
   ترشيحThe residue was filtered
2. 2
   أخرىthe filtrate was evaporated in vacuo to dryness
3. 3
   workup.DISSOLUTIONThe remaining product was dissolved
4. 4
   درجة الحرارةunder reflux in 400 ml ethyl acetate
5. 5
   ترشيحthe hot solution was filtered
6. 6
   أخرىthe mixture was subjected to a chromatographic purification (Florisil)
7. 7
   أخرىThe compound was then recrystallised from ethyl acetate

الإجراء التجريبي

12.31 g (107 mMol) N-hydroxysuccinimide and 22.70 g (110 mMol) dicyclohexylcarbodiimide were added at −35° C. to a solution of 18.27 g (107 mMol) (Pyrimidin-2-ylsulfanyl)-acetic acid (a) dissolved in 200 ml DMF. The reaction mixture was stirred for 16 h under argon. The residue was filtered and the filtrate was evaporated in vacuo to dryness. The remaining product was dissolved under reflux in 400 ml ethyl acetate, the hot solution was filtered and the mixture was subjected to a chromatographic purification (Florisil) using ethyl acetate. The compound was then recrystallised from ethyl acetate.

المصدر