Hydrochloric Acid → HCID 10543413、化合物

HRID 1197765ノート

反応式

HRID 1197765 の反応式
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

参加物

5

反応物 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

生成物 1

HCID 10543413HCID 10543413、化合物収率 81.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e78a591ac1964995a44978dae07ec2af
出典データセット
uspto-grants-1994_01
特許番号
US05278158

反応ノート

読み込み中…