Methyl 2-isocyanato-3-phenylpropanoate → HCID 178470451, 화합물

HRID 442341

반응식

HRID 442341 반응식
[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]

참가 물질

4

반응물 2

HCID 2769481Methyl 2-isocyanato-3-phenylpropanoateHCID 178470447HCID 178470447, 화합물

생성물 1

HCID 178470451HCID 178470451, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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.)

출처 및 근거

ORD 기록
ord-b2cc4793090c40cdb214bfcdf265bfe9
출처 데이터셋
uspto-grants-1977_08
특허 번호
US04045439

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