Dichloroacetyl chloride → Benoxacor

HRID 745886

反応式

HRID 745886 の反応式
[Cl:1][CH:2]([Cl:6])[C:3](Cl)=[O:4].[CH3:7][CH:8]1[NH:13][C:12]2[CH:14]=[CH:15][CH:16]=[CH:17][C:11]=2[O:10][CH2:9]1.C(=O)([O-])[O-].[Na+].[Na+]>C1C=CC=CC=1.O.C(OCC)(=O)C>[Cl:1][CH:2]([Cl:6])[C:3]([N:13]1[C:12]2[CH:14]=[CH:15][CH:16]=[CH:17][C:11]=2[O:10][CH2:9][CH:8]1[CH3:7])=[O:4]

参加物

7

反応物 3

HCID 6593Dichloroacetyl chlorideHCID 10340Sodium CarbonateHCID 27637603-Methyl-3,4-dihydro-2H-1,4-benzoxazine

生成物 1

HCID 62306Benoxacor収率 83%

試薬・触媒・溶媒 3

HCID 241Benzene溶媒HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

実験手順

5.3 ml (55 mmoles) of dichloroacetyl chloride are added dropwise, at a temperature of 20° to 25° C. and while stirring, to a suspension of 7.5 g (50 mmoles) of 2,3-dihydro-3-methyl-1,4-benzoxazine and 5.8 g (55 mmoles) of sodium carbonate in 120 ml of benzene. The reaction mixture is then stirred at the same temperature for 30 minutes and is then taken up in a mixture of water and ethyl acetate. The organic phase is washed with saturated sodium chloride solution, dried over sodium sulfate and evaporated. Crystallising the residue from diisopropyl ether gives 10.8 g of 4-dichloroacetyl-2,3-dihydro-3-methyl-1,4-benzoxazine, melting point 105°-107° C.

後処理

  1. washThe organic phase is washed with saturated sodium chloride solution
  2. dry with materialdried over sodium sulfate
  3. customevaporated
  4. customCrystallising the residue from diisopropyl ether

出典と根拠

ORDレコード
ord-575aa25dc6ff485985743d86433e5a8e
出典データセット
uspto-grants-1986_07
特許番号
US04601745

関連ノート

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