Pyridine → 2-[(3-Oxobutanoyl)amino]ethyl 2-methylprop-2-enoate

HRID 1903857

反応式

HRID 1903857 の反応式
N1C=CC=CC=1.Cl.[C:8]([O:13][CH2:14][CH2:15][NH2:16])(=[O:12])[C:9]([CH3:11])=[CH2:10].[CH2:17]=[C:18]1[O:22][C:20](=[O:21])[CH2:19]1>CN(C)C=O>[C:8]([O:13][CH2:14][CH2:15][NH:16][C:20](=[O:21])[CH2:19][C:18]([CH3:17])=[O:22])(=[O:12])[C:9]([CH3:11])=[CH2:10]

参加物

5

反応物 3

HCID 1049PyridineHCID 12661DiketeneHCID 75495Aminoethyl methacrylate hydrochloride

生成物 1

HCID 220239722-[(3-Oxobutanoyl)amino]ethyl 2-methylprop-2-enoate収率 60%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
20 °C

実験手順

Pyridine (16 g, 0.2 mole) was added dropwise at 0° C. to a solution of 2-aminoethyl methacrylate hydrochloride (33 g, 0.2 mole) and diketene (16.8 g, 0.2 mole) in N,N-dimethylformamide (600 ml). After the addition, the solution was stirred at 20° C. for 20 hours. The solvent was then removed at low vacuum. The residue was dissolved in chloroform (1200 ml), washed with water (twice with 200 ml), dried over anhydrous magnesium sulfate and filtered. Excess solvent was then removed. Distillation of the residue gave acetoacetamidoethyl methacrylate (b.p.=113°-132° C./5μ) at a yield of 60%.

後処理

  1. additionAfter the addition
  2. customThe solvent was then removed at low vacuum
  3. dissolutionThe residue was dissolved in chloroform (1200 ml)
  4. washwashed with water (twice with 200 ml),
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. customExcess solvent was then removed
  8. distillationDistillation of the residue

出典と根拠

ORDレコード
ord-42f0898122e24563af8593dc763dc62e
出典データセット
uspto-grants-1984_03
特許番号
US04438278

関連ノート

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