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Gyki 52895 → Acetamide, N-acetyl-N-(4-(7-acetyl-8,9-dihydro-8-methyl-7H-1,3-dioxolo(4,5-h)(2,3)benzodiazepin-5-yl)phenyl)-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Gyki 52895 | HCID 3539 | — |
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 生成物 | Acetamide, N-acetyl-N-(4-(7-acetyl-8,9-dihydro-8-methyl-7H-1,3-dioxolo(4,5-h)(2,3)benzodiazepin-5-yl)phenyl)- | HCID 3072682 | — |
反応手順
2.0 g (6.7 mmol) of 1-(4-aminophenyl)-4-methyl-7,8-methylenedioxy-3,4-dihydro-5H-2,3-benzodiazepine were refluxed with 40 ml of acetic anhydride for 3 hours, then it was evaporated to dryness under reduced pressure. The crystalline residue was transferred with 25 ml of water to a filter and washed with 5×3 ml of water. After drying 2.79 g of the raw triacetyl derivative were obtained. After washing with 20 ml of isopropanol and drying at 100° C. 2.39 g (84.6 of the pure aimed product were obtained, m.p. 224°-227° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05639751 |
| 出典データセット | uspto-grants-1997_06 |
| ORD ID | ord-30143e85f85a47d7ae9d70b80e34e758 |
| 出典メモ | uspto-grants-1997_06 |