تفاعل #3766
ord-46ef6b3fdcb74f75b3a22e357525e9cd
معادلة التفاعل
الكواشف
ظروف التفاعل
المعالجة
- 1أخرىrising to 41° C
- 2أخرىA thick, white suspension resulted
- 3درجة الحرارةheated at 45°-55° C. for 16 hours
- 4أخرىAfter ending of the reaction
- 5ترشيحthe solid was filtered off
- 6غسيلwashed with 2×3 ml of ethyl acetate
- 7أخرىThe combined filtrates were evaporated in vacuo
- 8غسيلthe semicrystalline residue which remained was washed
- 9أخرىThe white solid thus obtained
- 10ترشيحwas filtered off
- 11غسيلwashed with 2×3 ml of ethanol
- 12أخرىsucked dry
- 13غسيلwashed
- 14workup.STIRRINGby stirring with 10 ml of isopropanol
- 15ترشيحAfter filtering off
- 16غسيلwashing with 2×2 ml of isopropanol
- 17أخرىdrying in vacuo
الإجراء التجريبي
1.27 g (0.011 mol) of N-hydroxysuccinimide were initially introduced into 10 ml of ethyl acetate, a solution of 3.22 g (0.012 mol) of diphenyl chlorophosphate in 10 ml of ethyl acetate was added and then a solution of 2.53 g (0.025 mol) of triethylamine in 10 ml of ethyl acetate was added dropwise in the course of 10 minutes, the temperature rising to 41° C. A thick, white suspension resulted, which was treated with a solution of 0.6 g (0.01 mol) of acetic acid in 10 ml of ethyl acetate and heated at 45°-55° C. for 16 hours. After ending of the reaction, the solid was filtered off and washed with 2×3 ml of ethyl acetate. The combined filtrates were evaporated in vacuo and the semicrystalline residue which remained was washed by stirring with 20 ml of ethanol for 30 minutes. The white solid thus obtained was filtered off, washed with 2×3 ml of ethanol, sucked dry and then washed by stirring with 10 ml of isopropanol. After filtering off, washing with 2×2 ml of isopropanol and drying in vacuo, 1.1 g (70%) of white acetic acid succinimidyl ester were obtained.