関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | Bromomethyl acetate | HCID 68536 | — |
| 反応物 | 5-(N-Boc-amino)-5,7-dihydro-6H-dibez[b,d]azepin-6-one | HCID 11493548 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 5-amino-7-(methoxyacetyl)-5,7-dihydro-6H-dibenz[b,d]azepin-6-one hydrochloride | HCID 22312635 | — |
反応手順
A solution of 5-(N-Boc-amino)-5,7-dihydro-6H-dibenz[b,d]azepin-6-one (1.03, 3.08 mmol) (Example 7-E) in DMF was treated with Cs2CO3 (1.10 g, 3.39 mmol) and warmed to 60° C. To the reaction mixture was added bromomethyl acetate (0.321 ml, 3.39 mmol) (Aldrich) and stirring continued for 17 h. After cooling to 23° C. the mixture was diluted with CH2Cl2, washed with several portions of brine and dried over Na2SO4. The title compound was purified by chromatography (SiO2, CHCl3).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06849650B2 |
|---|
| 出典データセット | uspto-grants-2005_02 |
|---|
| ORD ID | ord-aa5db1a52ef141b09e1c109095bb69a8 |
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| 出典メモ | uspto-grants-2005_02 |
|---|
