Phosgene → Methyl 2-isocyano-3-phenylpropanoate

HRID 1974013

반응식

HRID 1974013 반응식
C(Cl)(Cl)=O.[CH3:5][O:6][C:7](=[O:19])[C@H:8]([CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[NH:9][CH:10]=O.CN1CCOCC1>C(Cl)Cl>[CH3:5][O:6][C:7](=[O:19])[CH:8]([N+:9]#[C-:10])[CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

참가 물질

5

반응물 3

HCID 6371PhosgeneHCID 79724-MethylmorpholineHCID 7016392N-formylphenylalanine methyl ester

생성물 1

HCID 2734779Methyl 2-isocyano-3-phenylpropanoate

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of phosgene (5.2 g, 0.052 mole) in dry methylene chloride (45 ml) is added dropwise to a stirred solution of N-formylphenylalanine methyl ester (10.0 g, 0.048 mole) and 1-methylmorpholine (13 g, 0.125 mole) in dry methylene chloride (25 ml) at -30° C. After completion of the addition the filtrate is concentrated under reduced pressure at room temperature. Benzene is added to the residue followed by filtration and concentration of the resulting solution. The residue is distilled to afford the title compound as a yellow oil, b.p. 97° C/0.3 mm, νmaxCHCl3 2150, 1746, 1595, 1578, 1489, 694 cm-1.

후처리

  1. additionAfter completion of the addition the filtrate
  2. concentrationis concentrated under reduced pressure at room temperature
  3. additionBenzene is added to the residue
  4. filtrationfollowed by filtration and concentration of the resulting solution
  5. distillationThe residue is distilled

출처 및 근거

ORD 기록
ord-700f229736794de7af45c62563758350
출처 데이터셋
uspto-grants-1976_12
특허 번호
US04000122

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