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Sodium Hydroxide → HCID 178526872, 화합물

HRID 1599683
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HRID 1599683 반응식
[OH-:1].[Na+].CC(O)(C)CN[C:7]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[N:10]2[N:17]=[N:18][N:19]=[C:9]2[C:8]=1[N+:20]([O-:22])=[O:21]>O>[N+:20]([C:8]1[C:9]2[N:10]([N:17]=[N:18][N:19]=2)[C:11]2[C:16]([C:7]=1[OH:1])=[CH:15][CH:14]=[CH:13][CH:12]=2)([O-:22])=[O:21]
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참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 154897582-Methyl-[(4-nitro-5-tetrazolo[1,5-a]quinolinyl)amino]-2-propanol

생성물 1

HCID 178526872HCID 178526872, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Aqueous sodium hydroxide (30 g of 50%) was added to a suspension of 2-methyl-[(4-nitro-5-tetrazolo[1,5-a]quinolinyl)amino]-2-propanol (34.0 g, 0.1125 mole, Example 3) in water (500 mL). The mixture was heated on a steam bath and the solid dissolved rapidly. The solution was heated for about 30 minutes and then upon stirring a solid began to precipitate. The mixture was made acidic with 6N hydrochloric acid. The resulting solid was isolated by filtration; washed in succession with water, ethanol and ether; then dried under vacuum at 100° C. to provide 23.2 g of crude product as a pale yellow/green solid. A sample (3.2 g) was recrystallized initially from methanol/dichloromethane and then from toluene to provide 4-nitrotetrazolo[1,5-a]quinolin-5-ol. Analysis: Calculated for C9H5N5O3 : % C, 46.76; % H, 2.18; % N, 30.29; Found: % C, 46.85; % H, 2.23; % N, 29.91.

후처리

  1. temperatureThe mixture was heated on a steam bath
  2. dissolutionthe solid dissolved rapidly
  3. temperatureThe solution was heated for about 30 minutes
  4. customto precipitate
  5. customThe resulting solid was isolated by filtration
  6. washwashed in succession with water, ethanol and ether
  7. customthen dried under vacuum at 100° C.
  8. customto provide 23.2 g of crude product as a pale yellow/green solid
  9. customA sample (3.2 g) was recrystallized initially from methanol/dichloromethane

출처 및 근거

ORD 기록
ord-0a28a4ccec4c46adb6aba9ae5e70817a
출처 데이터셋
uspto-grants-1998_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05741908

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