Benzoyl Peroxide → HCID 14888669、化合物

HRID 840135ノート

反応式

HRID 840135 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 14888669HCID 14888669、化合物

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-2f45f678453e4d1a8f6932654b944206
出典データセット
uspto-grants-2002_04
特許番号
US06365592B1

反応ノート

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