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Toluene → HCID 17929730、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 | Chloroform | HCID 6212 | — |
| 反応物 | Hexylamine | HCID 8102 | — |
| 反応物 | 1H,3H-Naphtho(1,8-cd)pyran-1,3-dione, 6-bromo- | HCID 66493 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | HCID 17929730 | HCID 17929730 | 74.3% |
反応手順
A mixture of 4-bromo-1,8-naphthalic anhydride (21.40 g, 77.2 mmol), n-hexylamine (13.1 mL, 100 mmol), toluene (200 mL), and chloroform (200 mL) was heated to boil for 1 hour. Precipitate formed making stirring difficult. The mixture was acidified with acetic acid, and heating was continued at 90° C. with distillation of chloroform. After all precipitate dissolved, the reaction mixture was poured onto crushed ice (300 g) and acidified with concentrated HCl to pH 1. After the ice melted, the solid was filtered off and dried. The crude product was purified by column chromatography (silica gel, hexane/ethyl acetate 2:1) to give 6-bromo-2-hexyl-1H-benzo[de]isoquinoline-1,3(2H)-dione (20.66 g, 74%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09382424B2 |
| 出典データセット | uspto-grants-2016_07 |
| ORD ID | ord-cb714efa8ddb440cbca5d203951d57bd |
| 出典メモ | uspto-grants-2016_07 |