Potassium Carbonate → Ethyl 2-{[di(tert-butoxycarbonyl)amino]methyl}acrylate

HRID 80598

반응식

HRID 80598 반응식
Br[CH2:2][C:3](=[CH2:9])[C:4]([O:6][CH2:7][CH3:8])=[O:5].[NH:10]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[C:21]([O:20][C:18]([N:10]([CH2:2][C:3](=[CH2:9])[C:4]([O:6][CH2:7][CH3:8])=[O:5])[C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])=[O:19])([CH3:24])([CH3:23])[CH3:22]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 279800Di-tert-butyl IminodicarboxylateHCID 3106202-(Bromomethyl)acrylic acid ethyl ester

생성물 1

HCID 86672207Ethyl 2-{[di(tert-butoxycarbonyl)amino]methyl}acrylate

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To ethyl 2-(bromomethyl)acrylate (104.4 g) in an acetonitrile (900 ml) solution, di-tert-butyl imino dicarboxylate (122.4 g) and potassium carbonate was added, and the mixture was stirred at room temperature for 2 days. The reaction solution was concentrated in vacuo. To the residue, ethyl acetate (1.4 liter) and water (700 ml) were added, and the layers were separated. The organic layer was washed with water (350 ml), dried over sodium sulfate, then concentrated to obtain ethyl 2-{[di(tert-butoxycarbonyl)amino]methyl}acrylate (compound S62a) as a crude product (182.7 g).

후처리

  1. concentrationThe reaction solution was concentrated in vacuo
  2. additionTo the residue, ethyl acetate (1.4 liter) and water (700 ml) were added
  3. customthe layers were separated
  4. washThe organic layer was washed with water (350 ml)
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-ffde7a9591174629b70fbf52587ce0f1
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846660B2

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