2-Chloro-4,6-diphenyl-1,3,5-triazine → 5-(4,6-Diphenyl-1,3,5-triazin-2-yl)-5,11-dihydro-11,11-dimethylindeno[1,2-b]carbazole

HRID 576458

反応式

HRID 576458 の反応式
[H-].[Na+].[CH3:3][C:4]1([CH3:24])[C:16]2[CH:15]=[C:14]3[C:17]4[C:22]([NH:23][C:13]3=[CH:12][C:11]=2[C:10]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]1=2)=[CH:21][CH:20]=[CH:19][CH:18]=4.Cl[C:26]1[N:31]=[C:30]([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[N:29]=[C:28]([C:38]2[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=2)[N:27]=1>ClCCl>[C:38]1([C:28]2[N:29]=[C:30]([C:32]3[CH:33]=[CH:34][CH:35]=[CH:36][CH:37]=3)[N:31]=[C:26]([N:23]3[C:13]4[C:14](=[CH:15][C:16]5[C:4]([CH3:24])([CH3:3])[C:5]6[CH:6]=[CH:7][CH:8]=[CH:9][C:10]=6[C:11]=5[CH:12]=4)[C:17]4[C:22]3=[CH:21][CH:20]=[CH:19][CH:18]=4)[N:27]=2)[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=1

参加物

5

反応物 3

HCID 196982-Chloro-4,6-diphenyl-1,3,5-triazineHCID 24758Sodium hydrideHCID 5805920311,11-Dimethyl-5,11-dihydroindeno[1,2-b]carbazole

生成物 1

HCID 665853465-(4,6-Diphenyl-1,3,5-triazin-2-yl)-5,11-dihydro-11,11-dimethylindeno[1,2-b]carbazole

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

1.5 g (37.5 mmol) of NaH (60% in oil) are initially introduced in 150 ml of dichloromethane. A solution of 8 g (28 mmol) of 12,12-dimethyl-6,12-dihydro-6-azaindeno[1,2-b]fluorene in dichloromethane is added dropwise at room temperature. After 1 h, 8.5 g (31 mmol) of 2-chloro-4,6-diphenyl-1,3,5-triazine are added dropwise, and the mixture is stirred at RT for 8 h. The solid which has precipitated out is recrystallised from toluene. The crystals which have deposited are filtered off with suction, washed with a little MeOH and dried in vacuo; yield: 11.6 g; 80% of theory; purity: 99.9% according to HPLC.

後処理

  1. customThe solid which has precipitated out
  2. customis recrystallised from toluene
  3. filtrationThe crystals which have deposited are filtered off with suction
  4. washwashed with a little MeOH
  5. customdried in vacuo

出典と根拠

ORDレコード
ord-5879785cf00c42a485ef382f11831e28
出典データセット
uspto-grants-2015_05
特許番号
US09040172B2

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