Water → HCID 86760639、化合物

HRID 900392

反応式

HRID 900392 の反応式
Cl.[Cl:2][C:3]1[CH:8]=[C:7]([Cl:9])[CH:6]=[CH:5][C:4]=1[NH:10][NH2:11].[CH3:12][CH:13]([C:19](=O)[C:20]([O:22][CH2:23][CH3:24])=[O:21])[C:14](OCC)=[O:15].C(O)(C(F)(F)F)=O.O>C1(C)C=CC=CC=1>[Cl:2][C:3]1[CH:8]=[C:7]([Cl:9])[CH:6]=[CH:5][C:4]=1[N:10]1[C:14](=[O:15])[CH:13]([CH3:12])[C:19]([C:20]([O:22][CH2:23][CH3:24])=[O:21])=[N:11]1

参加物

6

反応物 4

HCID 962WaterHCID 6422Trifluoroacetic acidHCID 97750Butanedioic acid, 2-methyl-3-oxo-, 1,4-diethyl esterHCID 2723905(2,4-Dichlorophenyl)hydrazine monohydrochloride

生成物 1

HCID 86760639HCID 86760639、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
75 °C

実験手順

2,4-dichlorophenylhydrazine hydrochloride(12.6 g) is dissolved in 100 ml of toluene and this solution is placed under nitrogen; after stirring, 10 g of diethyl 2-methyl-3-oxosuccinate are added and the mixture is then heated and 5 ml of TFA are added at 55° C. The mixture is left at the reflux of the solvent for 4 and a half hours, with stirring. The mixture is allowed to return to ambient temperature and is then heated to 75° C. and the reaction medium is hydrolyzed with 30 ml of water. The mixture is separated by settling out, the aqueous phase is discarded and the organic phase is then evaporated in order to eliminate the residual TFA. The organic phase is taken up with 10 ml of toluene and the expected product then crystallizes, m=10.2 g.

後処理

  1. temperaturethe mixture is then heated
  2. waitThe mixture is left at the
  3. temperaturereflux of the solvent for 4 and a half hours
  4. stirringwith stirring
  5. customto return to ambient temperature
  6. customThe mixture is separated
  7. customthe organic phase is then evaporated in order
  8. customthe expected product then crystallizes

出典と根拠

ORDレコード
ord-abe29720067d431584a668e3a7708b84
出典データセット
uspto-grants-2008_04
特許番号
US07358371B2

関連ノート

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