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

HRID 37118노트

반응식

HRID 37118 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ae7e2fa6f93645d18f2670d5ab1da1d7
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05420126

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