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

HRID 2277342ノート

反応式

HRID 2277342 の反応式
[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

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-089a2f96f3eb435d9530107b036be6ad
出典データセット
uspto-grants-2015_09
特許番号
US09133119B2

反応ノート

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