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

HRID 236621

反応式

HRID 236621 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-dbec6eb0f4ab429e85821da29e801d71
出典データセット
uspto-grants-1987_02
特許番号
US04645818

関連ノート

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