2-Acetonyloxy-4-chloro-3-fluoronitrobenzene → HCID 13188587、化合物

HRID 851084ノート

反応式

HRID 851084 の反応式
[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]

参加物

4

反応物 1

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

生成物 1

HCID 13188587HCID 13188587、化合物収率 75.5%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d37ce0e08bc44a22b7e9c6d5df77b00e
出典データセット
uspto-grants-1983_05
特許番号
US04382892

反応ノート

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