Hydrochloric Acid → HCID 86732791, 화합물

HRID 525924노트

반응식

HRID 525924 반응식
[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]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 23668193Sodium NitriteHCID 86732790HCID 86732790, 화합물

생성물 1

HCID 86732791HCID 86732791, 화합물수율 74.5%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

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

후처리

  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

출처 및 근거

ORD 기록
ord-7a91a269a61c4acea9f412832ec75af3
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09340556B2

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