Hydrochloric Acid → HCID 86732791、化合物

HRID 525924ノート

反応式

HRID 525924 の反応式
[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]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 23668193Sodium NitriteHCID 86732790HCID 86732790、化合物

生成物 1

HCID 86732791HCID 86732791、化合物収率 74.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

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

後処理

  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

出典と根拠

ORDレコード
ord-7a91a269a61c4acea9f412832ec75af3
出典データセット
uspto-grants-2016_05
特許番号
US09340556B2

反応ノート

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