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Toluene → HCID 178483721、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | 2,5-Dihydroxybenzaldehyde | HCID 70949 | — |
| 反応物 | 8-amino-2-[2-(dimethylamino)ethyl]-1H-dibenzo[de,h]isoquinoline-1,3(2H)-dione | HCID 10065414 | — |
| 溶媒 | Dichloromethane methanol | HCID 21226129 | — |
| 生成物 | HCID 178483721 | HCID 178483721 | 88.2% |
反応手順
A mixture of 50 mg (0.150 mmole) of 8-amino-2-[2-(dimethylamino)ethyl]-1H-dibenzo[de,h]isoquinoline-1,3(2H)-dione (obtained in example 4), 5 mL of toluene and 25 mg (1.2 molar equivalent) of 2,5-dihydroxybenzaldehyde was refluxed for 3 hours. After cooling, toluene was evaporated under reduced pressure and the residue was submitted to a flash chromatography on silica (eluent: CH2Cl2/methanol in a 95:5 and then a 90:10 volume ratio), thus resulting in 60 mg (yield: 88%) of the desired product (formula below) as a deep red powder.
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-8082caa1a5ca4d7e9e3f980915bf164d |
| 出典メモ | uspto-grants-2010_06 |