Methyl 2-isocyanato-3-phenylpropanoate → HCID 178470451、化合物

HRID 442341

反応式

HRID 442341 の反応式
[N:1]([CH:4]([C:12]([O:14][CH3:15])=[O:13])[CH2:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=[C:2]=[O:3].[NH2:16][C:17]1[CH:18]=[C:19]2[C:24](=[CH:25][CH:26]=1)[N:23]=[N:22][C:21]([C:27]([O:29][CH2:30][CH3:31])=[O:28])=[C:20]2[OH:32]>N1C=CC=CC=1>[OH:32][C:20]1[C:19]2[C:24](=[CH:25][CH:26]=[C:17]([NH:16][C:2]([NH:1][CH:4]([C:12]([O:14][CH3:15])=[O:13])[CH2:5][C:6]3[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=3)=[O:3])[CH:18]=2)[N:23]=[N:22][C:21]=1[C:27]([O:29][CH2:30][CH3:31])=[O:28]

参加物

4

反応物 2

HCID 2769481Methyl 2-isocyanato-3-phenylpropanoateHCID 178470447HCID 178470447、化合物

生成物 1

HCID 178470451HCID 178470451、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

1-Isocyanato-1-methoxycarbonyl-2-phenylethane (1.2 g.) was added to a stirred solution of ethyl 6-amino-4-hydroxycinnolin-3-yl carboxylate (1.17 g.) in pyridine (20 ml.). The mixture was stirred overnight and the solid which separated was washed successively with pyridine (10 ml.) and ether (100 ml.). The solid was dissolved in boiling ethanol (1 l.), and the solution was filtered whilst hot. The filtrate was evaporated to approximately 300 ml. After standing at 0° C. overnight, the mixture was filtered and the solid residue washed successively with ethanol (50 ml.) and ether (100 ml.) to give ethyl 4-hydroxy-6-[3-(α-methoxycarbonylphenethyl)ureido]cinnolin-3-yl carboxylate, m.p. 242°-243° C.

後処理

  1. customthe solid which separated
  2. washwas washed successively with pyridine (10 ml.) and ether (100 ml.)
  3. dissolutionThe solid was dissolved
  4. filtrationthe solution was filtered whilst hot
  5. customThe filtrate was evaporated to approximately 300 ml
  6. waitAfter standing at 0° C. overnight
  7. filtrationthe mixture was filtered
  8. washthe solid residue washed successively with ethanol (50 ml.) and ether (100 ml.)

出典と根拠

ORDレコード
ord-b2cc4793090c40cdb214bfcdf265bfe9
出典データセット
uspto-grants-1977_08
特許番号
US04045439

関連ノート

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