Water → 3-Bromo-8,8-dimethyl-8H-indolo[3,2,1-de]acridine

HRID 2277342노트

반응식

HRID 2277342 반응식
[CH3:1][C:2]1([CH3:22])[C:15]2[C:10]3=[C:11]([C:16]4[CH:17]=[CH:18][CH:19]=[CH:20][C:21]=4[N:9]3[C:8]3[CH:7]=[CH:6][CH:5]=[CH:4][C:3]1=3)[CH:12]=[CH:13][CH:14]=2.C1C(=O)N([Br:30])C(=O)C1.O>C(Cl)Cl.C(#N)C>[Br:30][C:18]1[CH:19]=[CH:20][C:21]2[N:9]3[C:8]4[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=4[C:2]([CH3:22])([CH3:1])[C:15]4[C:10]3=[C:11]([CH:12]=[CH:13][CH:14]=4)[C:16]=2[CH:17]=1

참가 물질

6

반응물 3

HCID 962WaterHCID 67184N-bromobutanimideHCID 125554028,8-dimethyl-8H-indolo[3,2,1-de]acridine

생성물 1

HCID 671095853-Bromo-8,8-dimethyl-8H-indolo[3,2,1-de]acridine

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 6344Dichloromethane용매

실험 절차

6.3 g (22.2 mmol) of 8,8-dimethylindolo[3,2,1-de]acridine are initially introduced in 150 ml of CH2Cl2. A solution of 3.9 g (22.3 mmol) of NBS in 100 ml of acetonitrile is subsequently added dropwise at −15° C. with exclusion of light, and the mixture is stirred at room temperature for a further 4 h. For work-up, 150 ml of water are added to the mixture, which is then extracted with CH2Cl2. The organic phase is dried over MgSO4, and the solvent is removed in vacuo. The product is washed by stirring with hot hexane and filtered off with suction.

후처리

  1. extractionis then extracted with CH2Cl2
  2. dry with materialThe organic phase is dried over MgSO4
  3. customthe solvent is removed in vacuo
  4. washThe product is washed
  5. stirringby stirring with hot hexane
  6. filtrationfiltered off with suction

출처 및 근거

ORD 기록
ord-089a2f96f3eb435d9530107b036be6ad
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09133119B2

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