N-bromobutanimide → HCID 9822596、化合物

HRID 1530910ノート

反応式

HRID 1530910 の反応式
[CH3:1][O:2][C:3]([C:5]1[C:9]([NH:10][S:11]([C:14]2[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=2)(=[O:13])=[O:12])=[CH:8][S:7][CH:6]=1)=[O:4].[Br:22]N1C(=O)CCC1=O>CC(O)=O.C(Cl)(Cl)Cl.CCOCC>[CH3:1][O:2][C:3]([C:5]1[C:9]([NH:10][S:11]([C:14]2[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=2)(=[O:13])=[O:12])=[C:8]([Br:22])[S:7][CH:6]=1)=[O:4]

参加物

5

反応物 2

HCID 67184N-bromobutanimideHCID 3542677HCID 3542677、化合物

生成物 1

HCID 9822596HCID 9822596、化合物収率 81%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 21584526Acetic acid chloroform溶媒

実験手順

To a solution of the product of Example 2 in 5.0 mL of AcOH-CHCl3 (1:1) at room temperature was added 0.299 g (1.682 mmol) of N-bromosuccinimide. The reaction was stirred for 18 h and then diluted with ether, washed with water and saturated sodium bicarbonate solution, dried over MgSO4, filtered and concentrated in vacuo. The tan solid residue was washed with ether-hexanes (1:1) to provide 0.504 g (81%) of the desired product as a tan solid. Electrospray Mass Spec:406.1 (M+H)+

後処理

  1. washwashed with water and saturated sodium bicarbonate solution
  2. dry with materialdried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. washThe tan solid residue was washed with ether-hexanes (1:1)

出典と根拠

ORDレコード
ord-5cd76b98a56a4783ad669611f7ccc8e0
出典データセット
uspto-grants-2001_03
特許番号
US06197795B1

反応ノート

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