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Formaldehyde → 1,4-Dibenzyl-6-benzyl-6-nitro-1,4-diazepane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | 1,2-Ethanediamine, N1,N2-bis(phenylmethyl)-, acetate (1:2) | HCID 31228 | — |
| 反応物 | 1-Nitro-2-phenylethane | HCID 80208 | — |
| 反応物 | Toluene methanol | HCID 21867641 | — |
| 生成物 | 1,4-Dibenzyl-6-benzyl-6-nitro-1,4-diazepane | HCID 58599847 | 89% |
反応手順
In a 250 mL round-bottom flask N,N′-dibenzylethylenediamine diacetate (19.67 g, 54.6 mmol) and 2-nitroethylbenzene (4, 8.28 g, 54.6 mmol) are dissolved in 1:1 toluene/methanol (100 mL). Paraformaldehyde (5.74 g, 0.191 mol) is added portion wise to the solution and the resulting suspension is refluxed. The mixture becomes homogeneous (dissolution of paraformaldehyde) and after 3 h at reflux, the mixture is cooled and evaporated in vacuo. The residue is recrystallized from methanol, obtaining pure 5 (20.29 g, 89%) as light yellow solid. M.p. 83-85° C. (EtOH), ESI-MS: 438 (MNa+), 416 (MH+); (Calc. for C26H29N3O2: 415 u.m.a.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08105567B2 |
| 出典データセット | uspto-grants-2012_01 |
| ORD ID | ord-613e51b5c25246efb9fbb35402fddf3f |
| 出典メモ | uspto-grants-2012_01 |