Water → HCID 178519561, 화합물

HRID 275259

반응식

HRID 275259 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 178519561HCID 178519561, 화합물수율 9%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-274805c1a99948e788ffde0c216112e5
출처 데이터셋
uspto-grants-1995_02
특허 번호
US05393730

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