氢氧化钾 → HCID 86732795，化合物

HRID 525927笔记

反应方程式

HRID 525927 反应方程式
[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]

参与物

5

反应物 2

HCID 14797氢氧化钾HCID 86732794HCID 86732794，化合物

产物 1

HCID 86732795HCID 86732795，化合物收率 64.5%

试剂、催化剂与溶剂 2

HCID 887Methanol溶剂HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

实验过程

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

后处理

  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

来源与证据

ORD记录
ord-a6068a94f2c54e33acaf161457cf625a
来源数据集
uspto-grants-2016_05
专利号
US09340556B2

反应笔记

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