Sodium Carbonate → 2-Bromo-7,7-dimethyl-5-phenyl-5,7-dihydroindeno[2,1-b]carbazole

HRID 2275911ノート

反応式

HRID 2275911 の反応式
[Br:1]N1C(=O)CCC1=O.[CH3:9][C:10]1([CH3:36])[C:18]2=[CH:19][C:20]3[N:21]([C:30]4[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=4)[C:22]4[C:27]([C:28]=3[CH:29]=[C:17]2[C:16]2[C:11]1=[CH:12][CH:13]=[CH:14][CH:15]=2)=[CH:26][CH:25]=[CH:24][CH:23]=4.C([O-])([O-])=O.[Na+].[Na+]>C(Cl)(Cl)Cl>[Br:1][C:25]1[CH:26]=[C:27]2[C:22](=[CH:23][CH:24]=1)[N:21]([C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1)[C:20]1[CH:19]=[C:18]3[C:10]([CH3:36])([CH3:9])[C:11]4[C:16]([C:17]3=[CH:29][C:28]2=1)=[CH:15][CH:14]=[CH:13][CH:12]=4

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 67184N-bromobutanimideHCID 6679800712,12-Dimethyl-10-phenyl-10,12-dihydro-10-azaindeno[2,1-b]fluorene

生成物 1

HCID 667976632-Bromo-7,7-dimethyl-5-phenyl-5,7-dihydroindeno[2,1-b]carbazole

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

9.51 g (54 mmol) of N-bromosuccinimide are added over the course of 15 min to a solution of 19.3 g (54 mmol) of 12,12-dimethyl-10-phenyl-10,12-dihydro-10-azaindeno[2,1-b]fluorene in 80 ml of chloroform at RT under a protective-gas atmosphere and with exclusion of light. The mixture is stirred for 6 h, 80 ml of sat. Na2CO3 soln. are subsequently added, and the organic phase is separated off and dried over Na2SO4. After removal of the solvent under reduced pressure, the residue is recrystallised, giving the product as a colourless solid in a yield of 20 g (45 mmol), 85%.

後処理

  1. additionare subsequently added
  2. customthe organic phase is separated off
  3. dry with materialdried over Na2SO4
  4. customAfter removal of the solvent under reduced pressure
  5. customthe residue is recrystallised

出典と根拠

ORDレコード
ord-c10f8ec23731447d9dc4fd12a4ae52d8
出典データセット
uspto-grants-2015_09
特許番号
US09126970B2

反応ノート

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