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

HRID 1903857

반응식

HRID 1903857 반응식
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]

참가 물질

5

반응물 3

HCID 1049PyridineHCID 12661DiketeneHCID 75495Aminoethyl methacrylate hydrochloride

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
20 °C

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-42f0898122e24563af8593dc763dc62e
출처 데이터셋
uspto-grants-1984_03
특허 번호
US04438278

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