P-Toluenesulfonylhydrazide → Methyl 2-chloro-3-(tosylhydrazono)butanoate

HRID 1721816ノート

反応式

HRID 1721816 の反応式
[Cl:1][CH:2]([C:7]([CH3:9])=O)[C:3]([O:5][CH3:6])=[O:4].[S:10]([NH:20][NH2:21])([C:13]1[CH:19]=[CH:18][C:16]([CH3:17])=[CH:15][CH:14]=1)(=[O:12])=[O:11]>C1COCC1.CCOCC>[Cl:1][CH:2]([C:7](=[N:21][NH:20][S:10]([C:13]1[CH:19]=[CH:18][C:16]([CH3:17])=[CH:15][CH:14]=1)(=[O:11])=[O:12])[CH3:9])[C:3]([O:5][CH3:6])=[O:4]

参加物

5

反応物 2

HCID 15303P-ToluenesulfonylhydrazideHCID 107332Methyl 2-chloroacetoacetate

生成物 1

HCID 73675184Methyl 2-chloro-3-(tosylhydrazono)butanoate

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of 25 ml of methyl 2-chloroacetoacetate in 25 ml of THF was added dropwise over 30 minutes to a solution of 37.5 g of tosyl hydrazine in 150 ml of THF. The mixture was allowed to stand overnight, then heated at reflux for 2 hours, cooled to room temperature and stripped of solvent. The residue was then dissolved in 200 ml of ether. Crystallization occurred at room temperature. The collected solids were dried to give methyl 2-chloro-3-(tosylhydrazono)butanoate (7B), as a light yellow solid, m.p.: 97°-101° C.

後処理

  1. temperatureheated
  2. temperatureat reflux for 2 hours
  3. customCrystallization
  4. customoccurred at room temperature
  5. customThe collected solids were dried

出典と根拠

ORDレコード
ord-fb73aa82c4234072abe40d9f77f5c2c3
出典データセット
uspto-grants-1989_08
特許番号
US04853027

反応ノート

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