Water → HCID 178519561、化合物

HRID 275259

反応式

HRID 275259 の反応式
[F:1][C:2]([F:21])([F:20])[C:3]1[CH:4]=[C:5]([CH:17]=[CH:18][CH:19]=1)[C:6]([C:8]1[N:16]=[CH:15][CH:14]=[CH:13][C:9]=1[C:10]([OH:12])=O)=[O:7].[Cl:22][C:23]1[CH:28]=[C:27]([C:29]([F:32])([F:31])[F:30])[CH:26]=[C:25]([Cl:33])[C:24]=1[NH:34][NH2:35].O>C1(C)C=CC=CC=1>[Cl:22][C:23]1[CH:28]=[C:27]([C:29]([F:31])([F:30])[F:32])[CH:26]=[C:25]([Cl:33])[C:24]=1[NH:34][N:35]=[C:10]([OH:12])[C:9]1[CH:13]=[CH:14][CH:15]=[N:16][C:8]=1[C:6](=[O:7])[C:5]1[CH:17]=[CH:18][CH:19]=[C:3]([C:2]([F:1])([F:21])[F:20])[CH:4]=1

参加物

5

反応物 3

HCID 962WaterHCID 688223[2,6-Dichloro-4-(trifluoromethyl)phenyl]hydrazineHCID 200788952-(3-Trifluoromethylbenzoyl)nicotinic acid

生成物 1

HCID 178519561HCID 178519561、化合物収率 9%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A suspension of 2-(3-trifluoromethylbenzoyl)nicotinic acid (1.5 g) and 2,6-dichloro-4-trifluoromethylphenylhydrazine (1.87 g) in toluene was stirred at reflux with azeotropic removal of water (using a Dean Stark apparatus) for 6.5 hours. The mixture was cooled to room temperature and then washed with 2N hydrochloric acid and water. The organic phase was dried and evaporated. The crude product was purified by column chromatography to yield a yellow gum which was triturated in hexane to yield the title compound as a pale yellow solid (0.24 g), m.p. 92°-96° C.

後処理

  1. customfor 6.5 hours
  2. washwashed with 2N hydrochloric acid and water
  3. customThe organic phase was dried
  4. customevaporated
  5. customThe crude product was purified by column chromatography
  6. customto yield a yellow gum which
  7. customwas triturated in hexane

出典と根拠

ORDレコード
ord-274805c1a99948e788ffde0c216112e5
出典データセット
uspto-grants-1995_02
特許番号
US05393730

関連ノート

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