N-bromobutanimide → HCID 9822596, 화합물

HRID 1530910노트

반응식

HRID 1530910 반응식
[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]

참가 물질

5

반응물 2

HCID 67184N-bromobutanimideHCID 3542677HCID 3542677, 화합물

생성물 1

HCID 9822596HCID 9822596, 화합물수율 81%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 21584526Acetic acid chloroform용매

실험 절차

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)+

후처리

  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)

출처 및 근거

ORD 기록
ord-5cd76b98a56a4783ad669611f7ccc8e0
출처 데이터셋
uspto-grants-2001_03
특허 번호
US06197795B1

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