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4-Methylmorpholine → HCID 66660968、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Methylmorpholine | HCID 7972 | — |
| 反応物 | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | (2S)-2-(((tert-butoxy)carbonyl)amino)-4-phenylbutanoic acid | HCID 7018726 | — |
| 反応物 | Methyl D-valinate hydrochloride | HCID 11984198 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 66660968 | HCID 66660968 | 142.3% |
反応手順
To an ice-cooled solution of D-valine methyl ester hydrochloride (1000 mg, 3.58 mmol) and HOBt (in DMF (14 mL) was added EDCI (755 mg, 3.94 mmol). After the mixture was stirred for 30 min, N-boc-L-homophenylalanine (600 mg, 3.58 mmol) and N-methylmorpholine (1 mL, 8.95 mmol) were added. The mixture was warmed to room temperature and stirred overnight. The solvent was removed and the residue was partitioned between water and EtOAc. The aqueous layer was extracted with EtOAc and the combined organic phases were dried over anhydrous Na2SO4. After concentration under reduced pressure, the crude title compound (2000 mg) was obtained and used in the next step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08022092B2 |
| 出典データセット | uspto-grants-2011_09 |
| ORD ID | ord-5fb008c1333246cdb0cbc165b6a859a0 |
| 出典メモ | uspto-grants-2011_09 |