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2,6-Dimethoxybenzoyl chloride → HCID 118308159、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,6-Dimethoxybenzoyl chloride | HCID 74810 | — |
| 反応物 | (1S,2S)-trans-N-Boc-1,2-cyclopentanediamine | HCID 17040218 | — |
| 反応物 | HCID 118308327 | HCID 118308327 | — |
| 生成物 | HCID 118308159 | HCID 118308159 | — |
反応手順
Prepared according to the procedure for N-[(1S,2R)-2-aminocyclopentyl]-2,6-dimethoxybenzamide hydrochloride (Intermediate 3) from tert-butyl N-[(1S,2S)-2-aminocyclopentyl]carbamate (CAS number 586961-34-4; 1.0 g, 4.99 mmol) and 2,6-dimethoxybenzoyl chloride (CAS number 1989-53-3; 1.50 g, 7.99 mmol) except that after the reaction was complete it was partitioned between DCM and a saturated solution of sodium bicarbonate, filtered through a hydrophobic frit and concentrated in vacuo. The Boc protected intermediate was purified by column chromatography (silica, 0-100% ethyl acetate/petrol) to give a white solid. After deprotection with HCl in 1,4-dioxane, azeotropic distillation from toluene afforded the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09156829B2 |
| 出典データセット | uspto-grants-2015_10 |
| ORD ID | ord-f54d203a12cf4e0da23faa0ddabeaa9d |
| 出典メモ | uspto-grants-2015_10 |