Pyridine → HCID 67770498, 화합물

HRID 259865

반응식

HRID 259865 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:11]=[CH:12][C:13]=1[O:14][CH3:15])[CH:6]=[CH:7][C:8](Cl)=[O:9].[NH2:16][C:17]1[C:18](=[O:37])[N:19]([CH3:36])[C:20]2[C:25]([C:26]=1[C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=1[Cl:33])=[CH:24][C:23]([CH3:34])=[CH:22][C:21]=2[CH3:35].N1C=CC=CC=1.C1COCC1>O>[OH2:2].[Cl:33][C:28]1[CH:29]=[CH:30][CH:31]=[CH:32][C:27]=1[C:26]1[C:25]2[C:20](=[C:21]([CH3:35])[CH:22]=[C:23]([CH3:34])[CH:24]=2)[N:19]([CH3:36])[C:18](=[O:37])[C:17]=1[NH:16][C:8](=[O:9])[CH:7]=[CH:6][C:5]1[CH:11]=[CH:12][C:13]([O:14][CH3:15])=[C:3]([O:2][CH3:1])[CH:4]=1

참가 물질

6

반응물 4

HCID 1049PyridineHCID 8028TetrahydrofuranHCID 22403900HCID 22403900, 화합물HCID 533992063,4-Dimethoxycinnamoylchloride

생성물 1

HCID 67770498HCID 67770498, 화합물수율 65.6%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 3,4-dimethoxycinnamoyl chloride (678 mg), 3-amino-4-(2-chlorophenyl)-1,6,8-trimethyl-2(1H)-quinolone (511 mg), pyridine (0.28 ml) and THF (10 ml) was stirred at room temperature for four days. Then, the mixture was diluted with water and extracted with ethyl acetate. The ethyl acetate layer was washed with water and dried (MgSO4). The solvent was removed and the residue was purified by a silica gel chromatography with benzene-acetone (4:1) to give crystals of 4-(2-chlorophenyl)-3-(3,4-dimethoxycinnamoylamino)-1,6,8-trimethyl-2(1H)-quinolone hydrate (510 mg, 65.6%). The crystals were recrystallized from ethanol to afford colorless prisms.

후처리

  1. extractionextracted with ethyl acetate
  2. washThe ethyl acetate layer was washed with water
  3. dry with materialdried (MgSO4)
  4. customThe solvent was removed
  5. customthe residue was purified by a silica gel chromatography with benzene-acetone (4:1)

출처 및 근거

ORD 기록
ord-e83d4e6373dc467487da94c93fa7144d
출처 데이터셋
uspto-grants-1996_06
특허 번호
US05523407

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