2-Iodoxybenzoic acid → 1-(4-Bromo-2-fluorophenyl)-2,2,2-trifluoroethan-1-one

HRID 880978

反応式

HRID 880978 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([OH:13])[C:9]([F:12])([F:11])[F:10])=[C:4]([F:14])[CH:3]=1.I(C1C=CC=CC=1C(O)=O)(=O)=O>C(OCC)(=O)C>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:13])[C:9]([F:12])([F:11])[F:10])=[C:4]([F:14])[CH:3]=1

参加物

4

反応物 2

HCID 1087942-Iodoxybenzoic acidHCID 616446351-(4-Bromo-2-fluorophenyl)-2,2,2-trifluoroethanol

生成物 1

HCID 669578641-(4-Bromo-2-fluorophenyl)-2,2,2-trifluoroethan-1-one収率 95.3%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 1-(4-bromo-2-fluorophenyl)-2,2,2-trifluoroethanol (1.09 g, 3.99 mmol) in ethyl acetate (30 mL) was added 2-iodoxybenzoic acid (2.28 g, 7.97 mmol). The reaction was heated to reflux overnight. The reaction was cooled to room temperature and diluted with heptanes (30 mL). The mixture was filtered through Celite and the filtrate was concentrated to give the title compound (1.03 g, 95%) as a pale yellow oil. 1H NMR (400 MHz, CDCl3, δ): 7.44 (dd, J=10.15, 1.56 Hz, 1H), 7.48 (m, 1H), 7.76 (m, 1H).

後処理

  1. temperatureThe reaction was heated
  2. temperatureto reflux overnight
  3. filtrationThe mixture was filtered through Celite
  4. concentrationthe filtrate was concentrated

出典と根拠

ORDレコード
ord-ee193e9496d840c59f80c6807398e0c3
出典データセット
uspto-grants-2015_03
特許番号
US08993586B2

関連ノート

読み込み中…