Diethyl 2-({4-[(acetyloxy)methyl]-2-iodoanilino}methylene)malonate → HCID 178469656, 화합물

HRID 1060596노트

반응식

HRID 1060596 반응식
[C:1]([O:4][CH2:5][C:6]1[CH:24]=[CH:23][C:9]([NH:10][CH:11]=[C:12]([C:18]([O:20]CC)=O)[C:13]([O:15][CH2:16][CH3:17])=[O:14])=[C:8]([I:25])[CH:7]=1)(=[O:3])[CH3:2]>O(C1C=CC=CC=1)C1C=CC=CC=1>[C:1]([O:4][CH2:5][C:6]1[CH:24]=[C:23]2[C:9](=[C:8]([I:25])[CH:7]=1)[N:10]=[CH:11][C:12]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[C:18]2[OH:20])(=[O:3])[CH3:2]

참가 물질

3

반응물 1

HCID 22724556Diethyl 2-({4-[(acetyloxy)methyl]-2-iodoanilino}methylene)malonate

생성물 1

HCID 178469656HCID 178469656, 화합물수율 62.2%

시약·촉매·용매 1

HCID 7583Diphenyl Ether용매

실험 절차

A solution of diethyl 2-({4-[(acetyloxy)methyl]-2-iodoanilino}methylene)malonate (1.75 g) in Ph2O (20 mL) is heated at 250° C. for 40 min. The reaction is cooled to room temperature and diluted with hexanes. The resulting solid is collected and dried. The crude solid is adsorbed onto silica and chromatographed (Biotage flash 40S, gradient from CH2CI2 to 2% MeOH/CH2Cl2). Product containing fractions are combined and concentrated to yield 0.98 g (62%) of ethyl 6-[(acetyloxy)methyl]-4-hydroxy-8-iodo-3-quinolinecarboxylate, m.p. 119-123° C.

후처리

  1. customThe resulting solid is collected
  2. customdried
  3. customchromatographed (Biotage flash 40S, gradient from CH2CI2 to 2% MeOH/CH2Cl2)
  4. additionProduct containing fractions
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-3fac58c96f704743b64d40026b37243d
출처 데이터셋
uspto-grants-2003_02
특허 번호
US06525049B2

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