Benzoyl Peroxide → HCID 14888669, 화합물

HRID 840135노트

반응식

HRID 840135 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([F:17])([F:16])[C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])=[CH:4][CH:3]=1.C1C(=O)N([Br:25])C(=O)C1.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>CCCCCC>[Br:25][CH2:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]([F:16])([F:17])[C:9]([O:11][C:12]([CH3:14])([CH3:13])[CH3:15])=[O:10])=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 7187Benzoyl PeroxideHCID 67184N-bromobutanimideHCID 109991821,1-Dimethylethyl α,α-difluoro-4-methylbenzeneacetate

생성물 1

HCID 14888669HCID 14888669, 화합물

시약·촉매·용매 1

HCID 8058Hexane용매

실험 절차

To tert butyl 2-{4-(methyl)phenyl}-2,2-difluoroacetate(see X. Creary, J. Org. Chem. 1987, 52, 5026) (4.8 g) in CC14 (80 mL) was added NBS (3.8 g), followed by benzoyl peroxide (100 mg). The reaction mixture was heated at reflux and was irradiated with a sun lamp for 1.5 h. The mixture was cooled down and diluted with hexane (50 mL) purified by filtration on a pad of silica gel. The filtrate was concentrated to give the title product for step 2 as a yellow-brown liquid (6.4 g) 1H NMR δ: (CD3COCD3), 1.48 (9H, m), 4.70 (2H, s), 7.62 (4H, m).

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux
  3. customwas irradiated with a sun lamp for 1.5 h
  4. temperatureThe mixture was cooled down
  5. filtrationpurified by filtration on a pad of silica gel
  6. concentrationThe filtrate was concentrated

출처 및 근거

ORD 기록
ord-2f45f678453e4d1a8f6932654b944206
출처 데이터셋
uspto-grants-2002_04
특허 번호
US06365592B1

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