Water → HCID 86760639, 화합물

HRID 900392

반응식

HRID 900392 반응식
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

참가 물질

6

반응물 4

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

생성물 1

HCID 86760639HCID 86760639, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
75 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-abe29720067d431584a668e3a7708b84
출처 데이터셋
uspto-grants-2008_04
특허 번호
US07358371B2

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