تفاعل #931191

معادلة التفاعل

1,4-Dioxa-spiro[4,5]decan-8-one

tosyl-methyl isocyanate

tBuOK

→

solid

المردود 67.7%

1,4-Dioxa-spiro[4,5]decane-8-carbonitrile

المردود 67.7%

المذيبات

dimethylformamide

water

ظروف التفاعل

المعالجة

1. 1
   استخلاصextracted with diethyl ether
2. 2
   غسيلThe combined extracts were washed with water and brine
3. 3
   تجفيفdried over MgSO4
4. 4
   ترشيحfiltered
5. 5
   تركيزconcentrated to a solid which
6. 6
   أخرىwas purified via flash chromatography on silica using 30% ethyl acetate/hexane as eluent

الإجراء التجريبي

To a solution of 1,4-Dioxa-spiro[4,5]decan-8-one (2.0 grams, 12.8 mmole) and tosyl-methyl isocyanate (5.0 grams, 25.6 mmole) in dimethylformamide (25 ml) at 0° C. was added 1.0 M tBuOK in tButanol (25.6 ml) and stirred at 0° C. for 1 hour and room temperature over night. The mixture was diluted with water and extracted with diethyl ether. The combined extracts were washed with water and brine, dried over MgSO4, filtered, and concentrated to a solid which was purified via flash chromatography on silica using 30% ethyl acetate/hexane as eluent to give a solid (1.45 g). MW 167.209; MS (m/e) 168 (M++1).

المصدر