Hydrochloric Acid → HCID 67051560、化合物

HRID 605697

反応式

HRID 605697 の反応式
F[C:2]1[CH:10]=[C:9]([F:11])[CH:8]=[C:7]([F:12])[C:3]=1[C:4]([OH:6])=[O:5].[F:13][C:14]1[CH:20]=[C:19]([I:21])[CH:18]=[CH:17][C:15]=1[NH2:16].[NH2-].[Li+].Cl>C(#N)C>[F:12][C:7]1[CH:8]=[C:9]([F:11])[CH:10]=[C:2]([NH:16][C:15]2[CH:17]=[CH:18][C:19]([I:21])=[CH:20][C:14]=2[F:13])[C:3]=1[C:4]([OH:6])=[O:5]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 24532Lithium amideHCID 1856942-Fluoro-4-iodoanilineHCID 5203732,4,6-Trifluorobenzoic acid

生成物 1

HCID 67051560HCID 67051560、化合物収率 59.2%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
60 °C

実験手順

2,4,6-Trifluorobenzoic acid (643 mg, 3.65 mmol) and 2-fluoro-4-iodoaniline (1.0 g, 4.22 mmol) were taken into acetonitrile (30 mL) followed by addition of lithium amide (290 mg, 12.7 mmol) and the mixture was heated to 60° C. under a nitrogen atmosphere for one hour. On cooling to room temperature the mixture was added to 1 N aqueous hydrochloric acid (100 mL) and the precipitate formed was collected by filtration and washed once with water then hexanes and dried in vacuo to give 2,4-difluoro-6-[(2-fluoro-4-iodophenyl)amino]benzoic acid (849 mg, 59% yield) as a tan solid. 1H-NMR (400 MHz, D6-DMSO): 13.72 (br s, 1H), 9.46 (s, 1H), 7.75 (d, 1H), 7.56 (d, 1H) 7.28 (tr, 1H), 6.73-6.67 (m, 1H), 6.53 (d, 1H).

後処理

  1. temperatureOn cooling to room temperature the mixture
  2. customthe precipitate formed
  3. filtrationwas collected by filtration
  4. washwashed once with water
  5. dry with materialhexanes and dried in vacuo

出典と根拠

ORDレコード
ord-0409980f7ea24b898c45b4a2ca38eb6b
出典データセット
uspto-grants-2011_03
特許番号
US07915250B2

関連ノート

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