化工社化工社 化学情報印刷レポート · 研究参考用
1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → CID 145857197
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| 反応物 | HOAt | HCID 181649 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | (S)-3-{[(benzyloxy)carbonyl][3-(trifluoromethyl)benzyl]amino}-4-oxo-4,6,7,8-tetrahydropyrrolo[1,2-a]pyrimidine-6-carboxylic Acid | HCID 57444827 | — |
| 反応物 | tert-butyl N-[4-(aminomethyl)benzenecarboximidoyl]carbamate | HCID 145832046 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | dichloromethane N,N-dimethylformamide | HCID 22350042 | — |
| 生成物 | CID 145857197 | HCID 145857197 | 79.2% |
反応手順
To a solution of intermediate 25a (0.281 mmol) and [(4-aminomethyl-phenyl)-imino-methyl]-carbamic acid tert-butyl ester (84 mg, 0.337 mmol) in 3 mL 5:1 CH2Cl2/DMF at 0° C., were added NaHCO3 (59 mg, 0.703 mmol), HOAT (42.1 mg, 0.309 mmol), and EDCI (75.5 mg, 0.393 mmol). The mixture was allowed to warm to rt and stir 20 h, then was diluted with EtOAc. The organic phase was washed with H2O, 1N HCl, H2O, and sat. NaHCO3, and brine, dried (Na2SO4) and brine. The crude residue was triturated with Et2O to afford 160 mg (79%) of intermediate 25b as a white solid. MS (ESI) 719.4 (M+H+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07094783B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-f36da15899fd4af9811f6c580396af9c |
| 出典メモ | uspto-grants-2006_08 |