2-Nitropropane → 3-Methyl-3-nitro-1,1,1-trifluorobutan-2-ol

HRID 36879

반응식

HRID 36879 반응식
C(O[CH:4]([OH:9])[C:5]([F:8])([F:7])[F:6])C.[N+:10]([CH:13]([CH3:15])[CH3:14])([O-:12])=[O:11].C(=O)([O-])[O-].[K+].[K+]>O>[CH3:14][C:13]([N+:10]([O-:12])=[O:11])([CH3:15])[CH:4]([OH:9])[C:5]([F:6])([F:7])[F:8]

참가 물질

5

반응물 3

HCID 3982-NitropropaneHCID 9897Ethanol, 1-ethoxy-2,2,2-trifluoro-HCID 11430Potassium Carbonate

생성물 1

HCID 199365423-Methyl-3-nitro-1,1,1-trifluorobutan-2-ol

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
65 °C

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)

후처리

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

출처 및 근거

ORD 기록
ord-dd1d05ae442b432398f97755dff0385d
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05418238

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