2-(Methylamino)ethanol → N-(2-methoxycarbonylphenyl)-N'-methyl-N'-(2-hydroxyethyl)urea

HRID 236621

반응식

HRID 236621 반응식
[CH3:1][O:2][C:3]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[N:11]=[C:12]=[O:13])=[O:4].[CH3:14][NH:15][CH2:16][CH2:17][OH:18]>C(OCC)(=O)C>[CH3:1][O:2][C:3]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[NH:11][C:12]([N:15]([CH3:14])[CH2:16][CH2:17][OH:18])=[O:13])=[O:4]

참가 물질

4

반응물 2

HCID 80162-(Methylamino)ethanolHCID 519494Methyl 2-isocyanatobenzoate

생성물 1

HCID 20216296N-(2-methoxycarbonylphenyl)-N'-methyl-N'-(2-hydroxyethyl)urea수율 72.5%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

A solution of 2-methoxycarbonyl phenylisocyanate (21.7 g) in ethyl acetate (116 g) is added dropwise to N-methylethanolamine (22.5 g), the mixture being stirred and cooled to keep the temperature below 36° C. The upper layer of the resulting mixture is separated and distilled at 60° C. under reduced pressure to remove ethyl acetate. The white solid residue remaining is triturated with ether, filtered, washed with ether and then dried in air to give N-(2-methoxycarbonylphenyl)-N'-methyl-N'-(2-hydroxyethyl)urea (22.4 g), m.pt. 90° C.

후처리

  1. temperaturecooled
  2. customthe temperature below 36° C
  3. customThe upper layer of the resulting mixture is separated
  4. distillationdistilled at 60° C. under reduced pressure
  5. customto remove ethyl acetate
  6. customThe white solid residue remaining is triturated with ether
  7. filtrationfiltered
  8. washwashed with ether
  9. customdried in air

출처 및 근거

ORD 기록
ord-dbec6eb0f4ab429e85821da29e801d71
출처 데이터셋
uspto-grants-1987_02
특허 번호
US04645818

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