O-Methylhydroxylamine hydrochloride → 6-cyano-3,4-dihydro-4-(5-methoxyimino-1-cyclopenten-1-yl)-2,2-dimethyl-2H-1,4-benzoxazine

HRID 37118ノート

反応式

HRID 37118 の反応式
[C:1]([C:3]1[CH:4]=[CH:5][C:6]2[O:11][C:10]([CH3:13])([CH3:12])[CH2:9][N:8]([C:14]3[C:18](=O)[CH2:17][CH2:16][CH:15]=3)[C:7]=2[CH:20]=1)#[N:2].Cl.[CH3:22][O:23][NH2:24]>N1C=CC=CC=1>[C:1]([C:3]1[CH:4]=[CH:5][C:6]2[O:11][C:10]([CH3:13])([CH3:12])[CH2:9][N:8]([C:14]3[C:18](=[N:24][O:23][CH3:22])[CH2:17][CH2:16][CH:15]=3)[C:7]=2[CH:20]=1)#[N:2]

参加物

4

反応物 2

HCID 521874O-Methylhydroxylamine hydrochlorideHCID 107306176-cyano-3,4-dihydro-2,2-dimethyl-4-(5-oxo-1-cyclopenten-1-yl)-2H-1,4-benzoxazine

生成物 1

HCID 539103166-cyano-3,4-dihydro-4-(5-methoxyimino-1-cyclopenten-1-yl)-2,2-dimethyl-2H-1,4-benzoxazine収率 78.2%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

In 3 ml of pyridine was dissolved 0.3 g of 6-cyano-3,4-dihydro-2,2-dimethyl-4-(5-oxo-1-cyclopenten-1-yl)-2H-1,4-benzoxazine followed by addition of 0.26 g of methoxyamine hydrochloride. The mixture was stirred at room temperature overnight and the solvent was then distilled off under reduced pressure. The residue was poured in water and extracted with ethyl acetate. The extract was washed with water and dried over anhydrous magnesium sulfate and the solvent was distilled Off under reduced pressure. Finally the residue was washed with ethanol-ether to give 0.26 g of 6-cyano-3,4-dihydro-4-(5-methoxyimino-1-cyclopenten-1-yl)-2,2-dimethyl-2H-1,4-benzoxazine.

後処理

  1. distillationthe solvent was then distilled off under reduced pressure
  2. additionThe residue was poured in water
  3. extractionextracted with ethyl acetate
  4. washThe extract was washed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationthe solvent was distilled Off under reduced pressure
  7. washFinally the residue was washed with ethanol-ether

出典と根拠

ORDレコード
ord-ae7e2fa6f93645d18f2670d5ab1da1d7
出典データセット
uspto-grants-1995_05
特許番号
US05420126

反応ノート

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