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Ethyl isothiocyanate → 1-{2-[2-(dimethylamino)ethyl]-1,3-dioxo-2,3-dihydro-1H-dibenzo[de,h]isoquinolin-11-yl}-3-[ethyl]thiourea
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl isothiocyanate | HCID 10966 | — |
| 反応物 | 11-amino-2-[2-(dimethylamino)ethyl]-1H-dibenzo[de,h]isoquinoline-1,3(2H)-dione | HCID 10065413 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 1-{2-[2-(dimethylamino)ethyl]-1,3-dioxo-2,3-dihydro-1H-dibenzo[de,h]isoquinolin-11-yl}-3-[ethyl]thiourea | HCID 16718042 | — |
反応手順
100 mg of 11-amino-2-[2-(dimethylamino)ethyl]-1H-dibenzo[de,h]isoquinoline-1,3(2H)-dione (obtained in example 3) (0.30 mmole) were dissolved in 6 ml of acetonitrile. 52 μl (2 molar equivalents) of ethyl isothiocyanate was added and the reaction mixture was maintained at room temperature for 16 hours. The solvent was then evaporated under reduced pressure and the residue was submitted to a flash chromatography (SiO2, CH2Cl2/MeOH 95/5). 92 mg of the desired product (formula shown hereinabove) were isolated as a red powder (yield=73%) 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-e94e0f6b38f94ec48d6d2f8474e9e84a |
| 出典メモ | uspto-grants-2010_06 |