Potassium Hydroxide → HCID 86732795, 화합물

HRID 525927노트

반응식

HRID 525927 반응식
[Cl:1][C:2]1[C:11]([O:12][CH2:13][C:14]2[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=2)=[C:10]([O:22][CH2:23][C:24]2[CH:29]=[CH:28][C:27]([O:30][CH3:31])=[CH:26][CH:25]=2)[CH:9]=[C:8]2[C:3]=1[C:4](=[O:46])[C:5]([C:34]([O:36]CC1C=CC(OC)=CC=1)=[O:35])=[N:6][N:7]2[CH2:32][CH3:33].[OH-].[K+]>CO.O>[Cl:1][C:2]1[C:11]([O:12][CH2:13][C:14]2[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=2)=[C:10]([O:22][CH2:23][C:24]2[CH:29]=[CH:28][C:27]([O:30][CH3:31])=[CH:26][CH:25]=2)[CH:9]=[C:8]2[C:3]=1[C:4](=[O:46])[C:5]([C:34]([OH:36])=[O:35])=[N:6][N:7]2[CH2:32][CH3:33]

참가 물질

5

반응물 2

HCID 14797Potassium HydroxideHCID 86732794HCID 86732794, 화합물

생성물 1

HCID 86732795HCID 86732795, 화합물수율 64.5%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

To the solution of 4-methoxybenzyl 5-chloro-1-ethyl-6,7-bis((4-methoxybenzyl)oxy)-4-oxo-1,4-dihydrocinnoline-3-carboxylate (24 g, 37.2 mmol) in methanol (400 mL) and water (133 mL) was added potassium hydroxide (8.35 g, 149 mmol). The reaction mixture was heated to reflux for 3 h. Solvent was removed under vacuum. The residue was suspended in water and the resulting mixture was acidified to pH4 with 2N hydrochloric acid. The precipitated solid was filtered and dried to afford 5-chloro-1-ethyl-6,7-bis((4-methoxybenzyl)oxy)-4-oxo-1,4-dihydrocinnoline-3-carboxylic acid (12.6 g, 24.00 mmol, 64.5% yield). LCMS: (M+H)+: 525.2

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 3 h
  3. customSolvent was removed under vacuum
  4. filtrationThe precipitated solid was filtered
  5. customdried

출처 및 근거

ORD 기록
ord-a6068a94f2c54e33acaf161457cf625a
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09340556B2

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