تفاعل #75618

معادلة التفاعل

tert-butyl 1,1-dichloro-2-oxo-7-azaspiro[3.5]nonane-7-carboxylate

ammonium chloride

→

tert-butyl 2-oxo-7-azaspiro[3.5]nonane-7-carboxylate

المردود 80.2%

المذيبات

methanol

ظروف التفاعل

المعالجة

1. 1
   ترشيحfiltered through Celite
2. 2
   أخرىThe filtrate was evaporated
3. 3
   workup.ADDITION1 N hydrochloric acid/ethyl acetate was added
4. 4
   أخرىthe organic layer was recovered
5. 5
   غسيلThe extract was washed with water, saturated sodium bicarbonate and brine
6. 6
   تجفيفdried over anhydrous magnesium sulfate
7. 7
   ترشيحfiltered
8. 8
   أخرىThe filtrate was evaporated

الإجراء التجريبي

106.1 g zinc dust was added to a mixture of 62.5 g tert-butyl 1,1-dichloro-2-oxo-7-azaspiro[3.5]nonane-7-carboxylate and 500 ml saturated ammonium chloride in methanol. The mixture was stirred for 1 hr and 20 min at room temperature and filtered through Celite. The filtrate was evaporated, 1 N hydrochloric acid/ethyl acetate was added thereto, and the organic layer was recovered. The extract was washed with water, saturated sodium bicarbonate and brine, dried over anhydrous magnesium sulfate, and filtered. The filtrate was evaporated, and the resulting residue was subjected to silica gel column chromatography to give 38.9 g of tert-butyl 2-oxo-7-azaspiro[3.5]nonane-7-carboxylate.

المصدر