반응 #64244

반응 방정식

ethyl acetate

acetic acid anhydride

formic acid

trans-4-nitroxycyclohexylamine

→

title compound

수율 66.4%

trans-N-formyl-4-nitroxycyclohexylamine

수율 66.4%

용매

water

반응 조건

후처리

1. 1
   온도is heated for 2 h to 60° C.
2. 2
   workup.ADDITIONmixed
3. 3
   기타One leaves
4. 4
   건조After neutralisation with saturated sodium hydrogen carbonate solution, the organic phase is dried with sodium sulphate
5. 5
   workup.DISTILLATIONdistilled off in a vacuum
6. 6
   여과After trituration with ether, the crystals are filtered off with suction

실험 절차

A mixture of 6.8 ml (0.072 mol) acetic acid anhydride and 2.8 ml (0.072 mol) formic acid is heated for 2 h to 60° C. and thereafter mixed, with cooling at 5° C., with 1.9 g (0.012 mol) trans-4-nitroxycyclohexylamine. One leaves to stir overnight at room temperature, subsequently dilutes with 100 ml ethyl acetate and adds 100 ml of water thereto. After neutralisation with saturated sodium hydrogen carbonate solution, the organic phase is dried with sodium sulphate and distilled off in a vacuum. After trituration with ether, the crystals are filtered off with suction. One obtains 1.5 g of the title compound of the m p 148°-150° C., i.e. 66% of theory.

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