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

HRID 1841526노트

반응식

HRID 1841526 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 CH2Cl2 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 CH2Cl2 to 2% MeOH/CH2Cl2)
  4. additionProduct containing fractions
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-7c42c9579730492294b0f84fe6defa9d
출처 데이터셋
uspto-grants-2004_01
특허 번호
US06683181B2

반응 노트

불러오는 중…