Hydrochloric Acid → HCID 10543413, 화합물

HRID 1197765노트

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HRID 1197765 반응식
C([NH:4][C:5]1[C:23]([N+:24]([O-:26])=[O:25])=[CH:22][C:8]2[N:9]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][N+:16]=3[O-:21])[CH2:10][C:11]([CH3:14])([CH3:13])[O:12][C:7]=2[CH:6]=1)(=O)C.Cl.C(=O)(O)[O-].[Na+]>C(O)C>[NH2:4][C:5]1[C:23]([N+:24]([O-:26])=[O:25])=[CH:22][C:8]2[N:9]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][N+:16]=3[O-:21])[CH2:10][C:11]([CH3:13])([CH3:14])[O:12][C:7]=2[CH:6]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 104985922-(7-acetamido-3,4-dihydro-2,2-dimethyl-6-nitro-2H-1,4-benzoxazin-4-yl)pyridine N-oxide

생성물 1

HCID 10543413HCID 10543413, 화합물수율 81.3%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
100 °C

실험 절차

To a suspension of 0.50 g 2-(7-acetamido-3,4-dihydro-2,2-dimethyl-6-nitro-2H-1,4-benzoxazin-4-yl)pyridine N-oxide in 6 ml ethanol, was added 6 ml of 5N HCl, the mixture was stirred at 100° C. for two hours, the reaction mixture was poured to ice water, and the resulting mixture was neutralized with sodium bicarbonate and extracted with chloroform. The extract was dried over anhydrous magnesium sulfate, the solvents were distilled off from the dried solution, and the residue thus obtained was recrystallized from ethanol, thus giving 359 mg of 2-(7-amino-3,4-dihydro-2,2-dimethyl-6-nitro-2H-1,4-benzoxazin-4-yl)pyridine N-oxide.

후처리

  1. extractionextracted with chloroform
  2. dry with materialThe extract was dried over anhydrous magnesium sulfate
  3. distillationthe solvents were distilled off from the dried solution
  4. customthe residue thus obtained
  5. customwas recrystallized from ethanol

출처 및 근거

ORD 기록
ord-e78a591ac1964995a44978dae07ec2af
출처 데이터셋
uspto-grants-1994_01
특허 번호
US05278158

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