반응 #65157

반응 방정식

triflouroacetaldehyde ethyl hemiacetal

2-nitropropane

potassium carbonate

→

3-methyl-3-nitro-1,1,1-trifluorobutan-2-ol

용매

water

반응 조건

후처리

1. 1
   workup.WAITfollowed by 2.5 days at room temperature
2. 2
   추출extracted with methylene chloride (100 ml+5×50 ml)
3. 3
   건조The combined organic layers are dried over sodium sulphate
4. 4
   기타the solvent is evaporated under reduced pressure
5. 5
   기타Purification of the liquid residue by flash chromatography on silica gel (eluant n-hexane/ethylacetate 85:15)

실험 절차

A mixture of triflouroacetaldehyde ethyl hemiacetal (2.58 ml), 2-nitropropane (1.81 ml) and potassium carbonate (111 mg) is stirred at 65° C. (oil bath temperature) for 6 hours followed by 2.5 days at room temperature. The reaction mixture is diluted with water (100 ml) and extracted with methylene chloride (100 ml+5×50 ml). The combined organic layers are dried over sodium sulphate and the solvent is evaporated under reduced pressure. Purification of the liquid residue by flash chromatography on silica gel (eluant n-hexane/ethylacetate 85:15) affords 3-methyl-3-nitro-1,1,1-trifluorobutan-2-ol as an oil (2.005 g)

출처