Nitromethane → Ethyl 4,4,4-trifluoro-3-(nitromethyl)butanoate

HRID 1360157

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HRID 1360157 반응식
[CH2:1]([O:3][C:4](=[O:11])[CH:5]=[CH:6][C:7]([F:10])([F:9])[F:8])[CH3:2].CN(C)C(N(C)C)=N.[N+:20]([CH3:23])([O-:22])=[O:21]>C(OC(=O)CC(C)=O)C>[CH2:1]([O:3][C:4](=[O:11])[CH2:5][CH:6]([CH2:23][N+:20]([O-:22])=[O:21])[C:7]([F:9])([F:10])[F:8])[CH3:2]

참가 물질

5

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온도
0 °C

실험 절차

1.0 g (5.94 mmol) of 4,4,4-trifluoro-2-butenoic acid ethyl ester and 0.15 mL (1.19 mmol) of 1,1,3,3-tetramethyl guanidine and 1.6 mL (29.8 mmol) of nitromethane were mixed. The resulting mixture was cooled to 0° C. and then stirred for 3 hours at room temperature, followed by addition of 100 mL of ethylacetoacetate. The reaction mixture was washed with water, and then an organic layer was dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to give 1.1 g (4.80 mmol) of the title compound in a yield of 81%.

후처리

  1. washThe reaction mixture was washed with water
  2. dry with materialan organic layer was dried over anhydrous magnesium sulfate
  3. distillationThe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-ebabf3d7f64247c4a01f2fcabda03b19
출처 데이터셋
uspto-grants-2011_02
특허 번호
US07879848B2

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