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

HRID 1360157ノート

反応式

HRID 1360157 の反応式
[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]

参加物

5

反応条件

温度
0 °C

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-ebabf3d7f64247c4a01f2fcabda03b19
出典データセット
uspto-grants-2011_02
特許番号
US07879848B2

反応ノート

読み込み中…