Hydrochloric Acid → 2-Chloroethyl 2-[(3-nitrophenyl)methylidene]-3-oxobutanoate

HRID 1284913ノート

反応式

HRID 1284913 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]([CH:9]=[CH:10][CH:11]=1)[CH:7]=O)([O-:3])=[O:2].[C:12]([O:18][CH2:19][CH2:20][Cl:21])(=[O:17])[CH2:13][C:14]([CH3:16])=[O:15].Cl>C1(C)C=CC=CC=1>[N+:1]([C:4]1[CH:5]=[C:6]([CH:9]=[CH:10][CH:11]=1)[CH:7]=[C:13]([C:14]([CH3:16])=[O:15])[C:12]([O:18][CH2:19][CH2:20][Cl:21])=[O:17])([O-:3])=[O:2]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 74493-NitrobenzaldehydeHCID 108605Butanoic acid, 3-oxo-, 2-chloroethyl ester

生成物 1

HCID 540552132-Chloroethyl 2-[(3-nitrophenyl)methylidene]-3-oxobutanoate

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

10 Grams of 3-nitrobenzaldehyde and 11 g of 2-chloroethyl acetoacetate were dissolved in 100 ml of toluene, then under an ice-cooled condition, hydrogen chloride gas was introduced into the solution for 2 hours. The reaction mixture was allowed to stand at room temperature for 2 days, and was concentrated. The residue obtained was extracted with chloroform, then the chloroform layer was washed with a saturated sodium chloride aqueous solution and with a saturated sodium hydrogen carbonate aqueous solution and dried with anhydrous magnesium sulfate. Chloroform was removed by distillation and the residue was recrystallized from isopropanol to yield 10 g of 2-chloroethyl 2-(3-nitrobenzyliden)acetoacetate in the form of colorless needle-like crystals.

後処理

  1. additionwas introduced into the solution for 2 hours
  2. concentrationwas concentrated
  3. customThe residue obtained
  4. extractionwas extracted with chloroform
  5. washthe chloroform layer was washed with a saturated sodium chloride aqueous solution and with a saturated sodium hydrogen carbonate aqueous solution
  6. dry with materialdried with anhydrous magnesium sulfate
  7. customChloroform was removed by distillation
  8. customthe residue was recrystallized from isopropanol

出典と根拠

ORDレコード
ord-ae2f417460a2403c8bbc65fb5b23a000
出典データセット
uspto-grants-1986_01
特許番号
US04564619

反応ノート

読み込み中…