2-Acetonyloxy-4-chloro-3-fluoronitrobenzene → HCID 13188587, 화합물

HRID 851084노트

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HRID 851084 반응식
[CH2:1]([O:5][C:6]1[C:11]([F:12])=[C:10]([Cl:13])[CH:9]=[CH:8][C:7]=1[N+:14]([O-])=O)[C:2]([CH3:4])=O>C(O)C.[Ni]>[Cl:13][C:10]1[CH:9]=[CH:8][C:7]2[NH:14][CH:2]([CH3:4])[CH2:1][O:5][C:6]=2[C:11]=1[F:12]

참가 물질

4

반응물 1

HCID 131885862-Acetonyloxy-4-chloro-3-fluoronitrobenzene

생성물 1

HCID 13188587HCID 13188587, 화합물수율 75.5%

시약·촉매·용매 2

HCID 935Nickel촉매HCID 702Ethanol용매

실험 절차

2.3 g (7.9 mmols) of 2-acetonyloxy-4-chloro-3-fluoronitrobenzene was dissolved in 30 ml of ethanol and catalytically reduced in the presence of 2 g of Raney nickel. After completion of the reduction, the catalyst was removed by filtration, and the filtrate was concentrated. The resulting residue was purified by silica gel (20 g) column chromatography using chloroform as an eluant to provide 1.2 g (75.5% yield) of 7-chloro-8-fluoro-3-methyl-2,3-dihydro-4H-1,4-benzoxazine as an oil.

후처리

  1. customAfter completion of the reduction, the catalyst was removed by filtration
  2. concentrationthe filtrate was concentrated
  3. customThe resulting residue was purified by silica gel (20 g) column chromatography

출처 및 근거

ORD 기록
ord-d37ce0e08bc44a22b7e9c6d5df77b00e
출처 데이터셋
uspto-grants-1983_05
특허 번호
US04382892

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