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Hydrochloric Acid → Tert-butyl 4-(4-(2-chloro-2-cyanovinyl)phenyl)piperazine-1-carboxylate

HRID 336841
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HRID 336841 반응식
O.NN.[CH:4]([C:6]1[CH:11]=[CH:10][C:9]([N:12]2[CH2:17][CH2:16][N:15]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH2:14][CH2:13]2)=[CH:8][CH:7]=1)=O.C(N(CC)CC)C.[Cl:32][C:33](Cl)(Cl)[C:34]#[N:35].Cl>CS(C)=O.[Cu]Cl>[Cl:32][C:33]([C:34]#[N:35])=[CH:4][C:6]1[CH:11]=[CH:10][C:9]([N:12]2[CH2:17][CH2:16][N:15]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH2:14][CH2:13]2)=[CH:8][CH:7]=1
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참가 물질

8

반응물 5

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 11011TrichloroacetonitrileHCID 24654Hydrazine hydrate (1:1)HCID 2795509Tert-butyl 4-(4-formylphenyl)piperazine-1-carboxylate

생성물 1

HCID 86671383Tert-butyl 4-(4-(2-chloro-2-cyanovinyl)phenyl)piperazine-1-carboxylate수율 26.6%

시약·촉매·용매 2

HCID 62652Cuprous chloride촉매HCID 679Dimethyl Sulfoxide용매3회

실험 절차

To a solution of hydrazine hydrate diluted in 16 ml of dimethylsulfoxide under argon are added dropwise a solution of 4.76 g (16.41 mmol) of tert-butyl 4-(4-formylphenyl)piperazine-1-carboxylate dissolved in 32 ml of dimethylsulfoxide. The reaction mixture is stirred at room temperature for 3 h before being cooled over an ice bath. Then, the successive addition is made of 11.45 ml (82 mmol) of triethylamine, 162 mg of copper (I) chloride and, in 5 min, a solution of 8.23 ml (82 mmol) of trichloroacetonitrile diluted in 16 ml of dimethylsulfoxide. The reaction mixture is stirred at room temperature for 18 h then poured onto an aqueous 0.1N hydrochloric acid solution. The product is extracted several times with dichloromethane. The organic phases are combined, dried over magnesium sulfate, and concentrated. The residue is purified by chromatography on silica (cyclohexane/ethyl acetate eluent: 8:2) to yield 1.52 g (26%) of tert-butyl 4-(4-(2-chloro-2-cyanovinyl)phenyl)piperazine-1-carboxylate in the form of a yellow solid (mixture of the two isomers Z/E).

후처리

  1. temperaturebefore being cooled over an ice bath
  2. additionThen, the successive addition
  3. stirringThe reaction mixture is stirred at room temperature for 18 h
  4. extractionThe product is extracted several times with dichloromethane
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated
  7. customThe residue is purified by chromatography on silica (cyclohexane/ethyl acetate eluent: 8:2)

출처 및 근거

ORD 기록
ord-346a03a009ad4e659dcb0eb89eabc413
출처 데이터셋
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08889711B2

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