盐酸 → HCID 86732791，化合物

HRID 525924笔记

反应方程式

HRID 525924 反应方程式
[NH2:1][C:2]1[C:11]2[O:12][CH2:13][O:14][C:10]=2[CH:9]=[C:8]2[C:3]=1[C:4](=[O:20])[C:5]([C:17]([OH:19])=[O:18])=[N:6][N:7]2[CH2:15][CH3:16].[N:21]([O-])=O.[Na+].[ClH:25]>O>[Cl-:25].[C:17]([C:5]1[C:4](=[O:20])[C:3]2[C:2]([N+:1]#[N:21])=[C:11]3[O:12][CH2:13][O:14][C:10]3=[CH:9][C:8]=2[N:7]([CH2:15][CH3:16])[N:6]=1)([OH:19])=[O:18]

参与物

5

反应物 3

HCID 313盐酸HCID 23668193亚硝酸钠HCID 86732790HCID 86732790，化合物

产物 1

HCID 86732791HCID 86732791，化合物收率 74.5%

试剂、催化剂与溶剂 1

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂2 次

实验过程

A mixture of 5-amino-1-ethyl-4-oxo-1,4-dihydro-[1,3]dioxolo[4,5-g]cinnoline-3-carboxylic acid (3.6 g, 12.99 mmol) in hydrochloric acid (conc) (20 ml) was stirred at room temperature and sodium nitrite (0.986 g, 14.28 mmol) in water (7 mL) was added dropwise to maintain the temperature bellow 45° C. Stirring continued for 5 h. The solution was poured into 50 ml of water and was allowed to stand overnight in the refrigerator. Precipitate was collected by filtration and dried over drierite in a desiccator to yield 3-Carboxy-1-ethyl-4-oxo-1,4-dihydro-[1,3]dioxolo[4,5-g]cinnoline-5-diazonium chloride (3.15 g, 9.67 mmol, 74.5% yield). LCMS: (M+H)+: 326.2

后处理

  1. temperatureto maintain the temperature bellow 45° C
  2. stirringStirring
  3. waitto stand overnight in the refrigerator
  4. filtrationPrecipitate was collected by filtration
  5. dry with materialdried over drierite in a desiccator

来源与证据

ORD记录
ord-7a91a269a61c4acea9f412832ec75af3
来源数据集
uspto-grants-2016_05
专利号
US09340556B2

反应笔记

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