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Benzyl chloroformate → (2,6-Dimethyl-4-morpholin-4-yl-phenyl)-carbamic acid benzyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzyl chloroformate | HCID 10387 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 2,6-Dimethyl-4-morpholin-4-yl-phenylamine | HCID 23009414 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | (2,6-Dimethyl-4-morpholin-4-yl-phenyl)-carbamic acid benzyl ester | HCID 11508357 | 47% |
反応手順
Benzyl chloroformate (32 mg) was added to a solution of 0.15 M 2,6-dimethyl-4-morpholin-4-yl-phenylamine and 0.30 M N,N-diisopropyl-ethylamine in 1,2-dichloroethane (1 mL). The vial was shaken for 16 hours and concentrated in vacuo. Aqueous sodium hydroxide (1 M, 2 mL) was added and the crude mixture was extracted with isopropyl acetate/tetrahydrofuran (4:1, 2.5 mL). The organic phase was concentrated in vacuo and redissolved in dimethyl sulfoxide (0.5 mL) of which 0.2 mL was subjected to preparative LC-MS purification to furnish 9.5 mg (47% yield) of the title compound as an oil. LC-MS (m/z) 341 (MH+); tR=2.28, (UV, ELSD) 100%, 100%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08012962B2 |
| 出典データセット | uspto-grants-2011_09 |
| ORD ID | ord-9759227e99734243b73ec7539d960962 |
| 出典メモ | uspto-grants-2011_09 |