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

HRID 711093

反応式

HRID 711093 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-2640f2ca716a4496b7a81e253e79dbf7
出典データセット
uspto-grants-2015_11
特許番号
US09181252B2

関連ノート

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