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Hydrochloric Acid → 8-chloro-10,11-dihydro-10-[(1,3-dihydro-1,3-dioxo-2H-isoindol-2-yl)acetyl]dibenz[b,f][1,4]oxazepine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2H-Isoindole-2-acetyl chloride, 1,3-dihydro-1,3-dioxo- | HCID 81242 | — |
| 反応物 | 8-Chloro-10,11-dihydrodibenzo[b,f][1,4]oxazepine | HCID 15229227 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 8-chloro-10,11-dihydro-10-[(1,3-dihydro-1,3-dioxo-2H-isoindol-2-yl)acetyl]dibenz[b,f][1,4]oxazepine | HCID 10669729 | — |
反応手順
1,3-dihydro-1,3-dioxo-2H-isoindole-2-acetyl chloride (4.00 grams), 8-chloro-10,11-dihydrodibenz[b,f][1,4]oxazepine (4.16 grams) and triethylamine (2.8 mL) were refluxed in toluene (100 mL) under nitrogen for 3 hours. The resulting mixture was poured into 1N HCl at 0° C., and the biphasic mixture was shaken vigorously. The insoluble product was collected by filtration, washed with toluene and ethyl ether, and dried in vacuo at 56° C. The yield of the title compound was 6.36 grams (85%). Mp: 184°-185° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05212169 |
| 出典データセット | uspto-grants-1993_05 |
| ORD ID | ord-9756dccc208d4fa6826e9969be32adff |
| 出典メモ | uspto-grants-1993_05 |