ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

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

HRID 336841
ノート
印刷プレビュー

反応式

HRID 336841 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 62652Cuprous chloride触媒HCID 679Dimethyl Sulfoxide溶媒3 回

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-346a03a009ad4e659dcb0eb89eabc413
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08889711B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート