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Tert-butyl N-[(4-cyanophenyl)methyl]-N-[(2-methylpropan-2-yl)oxycarbonyl]carbamate → 4-(Aminomethyl)benzonitrile hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tert-butyl N-[(4-cyanophenyl)methyl]-N-[(2-methylpropan-2-yl)oxycarbonyl]carbamate | HCID 3683768 | — |
| 反応物 | 1,4-Dioxane hydrochloride | HCID 20443148 | — |
| 生成物 | 4-(Aminomethyl)benzonitrile hydrochloride | HCID 9942250 | — |
反応手順
4-cyanobenzylamine hydrochloride (EX-59A) was prepared from 10 g (0.030 moles) of 4-{N,N-bis-(tert-butoxycarbonyl)aminomethyl}benzonitrile, prepared following Synthetic Communication, 28(23), 4419-4429 (1998), by stirring it in 4N HCl Dioxane (75 ml). After 3 h, the solution was concentraed in vacuo and triturated with ether. The solid was collected by filtration and vacuum dried to yield 5 g (98%) of EX-59A as a white solid: 1H NMR (DMSO) d 8.68 (br s, 2H) 7.84 (m, 2H), 7.67 (m, 2H), 4.06 (s, 2H); HRMS (EI) calcd for C8H8N2 133.0766, found 133.0807.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06664255B1 |
| 出典データセット | uspto-grants-2003_12 |
| ORD ID | ord-a94ce1e362de4d3bad6b881d570b3162 |
| 出典メモ | uspto-grants-2003_12 |