化工社化工社 化学情報印刷レポート · 研究参考用
1,2-Dichloroethane → (2R)-2-(morpholine-4-carbonyl)-pyrrolidine-1-carboxylic acid tert-butyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,2-Dichloroethane | HCID 11 | — |
| 反応物 | Morpholine | HCID 8083 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | (2R)-1-[(tert-butoxy)carbonyl]pyrrolidine-2-carboxylic acid | HCID 688022 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (2R)-2-(morpholine-4-carbonyl)-pyrrolidine-1-carboxylic acid tert-butyl ester | HCID 69832143 | 63% |
反応手順
(2R)-Pyrrolidine-1,2-dicarboxylic acid 1-tert-butyl ester (2.15 g, 10 mmol) reacted with morpholine (1.3 mL, 15 mmol) in CH2Cl2 (30 mL) in the presence EDC (2.7 g, 15 mmol), HOBT (1.9 g, 15 mmol) and Et3N (2.1 mL, 15 mmol) at r.t. for 14 h. The mixture was evaporated to dryness and purified by column chromatography. After washing the resulting solid with aqueous NaHCO3 followed by H2O to remove HOBT contamination, pure compound (2R)-2-(morpholine-4-carbonyl)-pyrrolidine-1-carboxylic acid tert-butyl ester 11a (1.79 g, 63%) was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06642232B2 |
| 出典データセット | uspto-grants-2003_11 |
| ORD ID | ord-cb98b0ab204440b8b8bbdb6d68f3c7fd |
| 出典メモ | uspto-grants-2003_11 |