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4-Chlorophenylacetyl chloride → 2-(4-chlorophenyl)-N-{2-[2-(dimethylamino)ethyl]-1,3-dioxo-2,3-dihydro-1H-dibenzo[de,h]isoquinolin-11-yl}acetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Chlorophenylacetyl chloride | HCID 90692 | — |
| 反応物 | 11-amino-2-[2-(dimethylamino)ethyl]-1H-dibenzo[de,h]isoquinoline-1,3(2H)-dione | HCID 10065413 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-(4-chlorophenyl)-N-{2-[2-(dimethylamino)ethyl]-1,3-dioxo-2,3-dihydro-1H-dibenzo[de,h]isoquinolin-11-yl}acetamide | HCID 16717840 | 84% |
反応手順
A solution of 100 mg (0.30 mmole) of 11-amino-2-[2-(dimethylamino)ethyl]-1H-dibenzo[de,h]isoquinoline-1,3(2H)-dione (obtained in example 3) in 7 mL of dichloromethane was magnetically stirred at 20° C. 113 μL (2 molar equivalents) of 4-chlorophenylacetyl chloride were added. The mixture was magnetically stirred at room temperature during 3 hours. The solvent was then evaporated under reduced pressure and the residue was submitted to a flash chromatography on silica (eluent: CH2Cl2/methanol in a 97:3 volume ratio) to provide 122 mg (yield: 84%). of the desired product (formula above) as an orange powder which was characterized as follows:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07741337B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-de30689099b04dcc8fd2962cf92b9651 |
| 出典メモ | uspto-grants-2010_06 |