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Acetic Anhydride → 2-(1-Acetamidocyclopentyl)acetic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 2-(1-Aminocyclopentyl)acetic acid | HCID 16212493 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-(1-Acetamidocyclopentyl)acetic acid | HCID 45119264 | — |
反応手順
Triethylamine (1.2 mL, 8.4 mmol), acetic anhydride (0.8 mL, 8.4 mL) and DMAP (10 mg, 0.09 mmol) are subsequentially added to a suspension of (1-amino-cyclopentyl)-acetic acid (1.00 g, 5.6 mmol) in THF (30 mL). After heating at 60° C. for 2 h AcOEt is added and the organic phase is washed with 1N HCl. Drying (Na2SO4), filtration and evaporation of the solvent yields the desired product. MS (LC-MS): [M+H]+=186.1. tR (HPLC, Waters Symmetry C18 column, 80-95% CH3CN/H2O/3.5 min, 95% CH3CN/H2O, 2 min, CH3CN and H2O containing 0.1% TFA, flow: 0.6 mL/min): 0.53 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07807709B2 |
| 出典データセット | uspto-grants-2010_10 |
| ORD ID | ord-226b45a4f01f412bbf58037929ca6e4d |
| 出典メモ | uspto-grants-2010_10 |