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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
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Chloro-4,6-diphenyl-1,3,5-triazine | HCID 19698 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 11,11-Dimethyl-5,11-dihydroindeno[1,2-b]carbazole | HCID 58059203 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 5-(4,6-Diphenyl-1,3,5-triazin-2-yl)-5,11-dihydro-11,11-dimethylindeno[1,2-b]carbazole | HCID 66585346 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09040172B2 |
| 出典データセット | uspto-grants-2015_05 |
| ORD ID | ord-5879785cf00c42a485ef382f11831e28 |
| 出典メモ | uspto-grants-2015_05 |