化工社化工社 化学情報印刷レポート · 研究参考用
Dicyclohexylcarbodiimide → (+/-)-N-(2-(dimethylamino)-3-{[(1,1-dimethylethyl)(dimethyl)silyl]oxy}-2-methyl-1-phenylpropyl)-2,3-dimethylbenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dicyclohexylcarbodiimide | HCID 10868 | — |
| 反応物 | 2,3-Dimethylbenzoic acid | HCID 11782 | — |
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | [2-Amino-1-({[(1,1-dimethylethyl)(dimethyl)silyl]oxy}methyl)-1-methyl-2-phenylethyl]dimethylamine | HCID 68562132 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (+/-)-N-(2-(dimethylamino)-3-{[(1,1-dimethylethyl)(dimethyl)silyl]oxy}-2-methyl-1-phenylpropyl)-2,3-dimethylbenzamide | HCID 68563699 | 30% |
反応手順
The title compound (64 mg; 30%) was prepared from [2-amino-1-({[(1,1-dimethylethyl)(dimethyl)silyl]oxy}methyl)-1-methyl-2-phenylethyl]dimethylamine D48 (150 mg; 0.46 mmol), 2,3-dimethylbenzoic acid (75 mg; 0.5 mmol), PL-dicyclohexylcarbodiimide (385 mg; 0.5 mmol; Polymer Labs 1.3 mmol/g), 1-hydroxybenzotriazole (77 mg; 0.5 mmol) in DCM (5 ml) in a similar manner to that described in E1. Mass spectrum (Electrospray LC/MS): Found 455 (MH+), C27H42N2O2Si requires 454. Ret. time 2.57 and 2.61 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07745642B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-3062e35499a94467b03248e37a763eba |
| 出典メモ | uspto-grants-2010_06 |