Sodium Trifluoroacetate → 3-Benzyloxy-6-trifluoromethyl-2-nitrotoluene

HRID 565001ノート

反応式

HRID 565001 の反応式
[CH2:1]([O:8][C:9]1[C:10]([N+:17]([O-:19])=[O:18])=[C:11]([CH3:16])[C:12](Br)=[CH:13][CH:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[F:20][C:21]([F:26])([F:25])C([O-])=O.[Na+]>[Cu]I.CN1CCCC1=O>[CH2:1]([O:8][C:9]1[C:10]([N+:17]([O-:19])=[O:18])=[C:11]([CH3:16])[C:12]([C:21]([F:26])([F:25])[F:20])=[CH:13][CH:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

5

反応物 2

HCID 517019Sodium TrifluoroacetateHCID 21194170HCID 21194170、化合物

生成物 1

HCID 105430343-Benzyloxy-6-trifluoromethyl-2-nitrotoluene

試薬・触媒・溶媒 2

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)触媒HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
160 °C

実験手順

A mixture of 1.50 g (4.66 mmol) of 3-benzyloxy-6-bromo-2-nitrotoluene, 6.33 g (46.6 mmol) of sodium trifluoroacetate, 4.43 g (23.3 mmol) of copper (I) iodide and 80 ml of N-methylpyrrolidone was heated at 160° C. for 7 hours while stirring. Next, the solvent was distilled off under reduced pressure and ethyl acetate was added to the resulting residue. Insoluble matters were then filtered off. The filtrate was washed twice with water. After drying over anhydrous magnesium sulfate, the solvent was distilled off under reduced pressure and the residue was isolated and purified by silica gel column chromatography to give 0.70 (48.3%) of 3-benzyloxy-6-trifluoromethyl-2-nitrotoluene.

後処理

  1. distillationNext, the solvent was distilled off under reduced pressure and ethyl acetate
  2. additionwas added to the resulting residue
  3. filtrationInsoluble matters were then filtered off
  4. washThe filtrate was washed twice with water
  5. dry with materialAfter drying over anhydrous magnesium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. customthe residue was isolated
  8. custompurified by silica gel column chromatography

出典と根拠

ORDレコード
ord-a7e9e7777e194a9b98249cb919663a5e
出典データセット
uspto-grants-2001_01
特許番号
US06169107A

反応ノート

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