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

HRID 1067787노트

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HRID 1067787 반응식
[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

참가 물질

5

반응물 2

HCID 517019Sodium TrifluoroacetateHCID 21194170HCID 21194170, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)촉매HCID 13387N-methyl-2-pyrrolidone용매

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온도
160 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6d0f4130c9c14d748364b85191d8f526
출처 데이터셋
uspto-grants-2001_06
특허 번호
US06248772B1

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