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Methanol → 9,10-dihydro-4H-pyrrolo[1,2-a]thieno[2,3-e][1,4]diazepine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Boron, trihydro(thiobis(methane))-, (T-4)- | HCID 9833925 | — |
| 反応物 | 9-oxo-9,10-dihydro-4H-pyrrolo[1,2-a]-thieno[2,3-e][1,4]diazepine | HCID 11041864 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 9,10-dihydro-4H-pyrrolo[1,2-a]thieno[2,3-e][1,4]diazepine | HCID 21837159 | — |
反応手順
To a mixture of 7.0 g of 9-oxo-9,10-dihydro-4H-pyrrolo[1,2-a]thieno[2,3-e][1,4]diazepin in 25 ml of anhydrous tetrahydrofuran is added 9 ml of 10 molar boron-dimethylsulfide in tetrahydrofuran. The mixture is refluxed for 6 hours. The solution is cooled to room temperature and 25 ml of methanol added dropwise. The volatiles are removed under vacuum. To the residue is added 100 ml of 2N NaOH. The mixture is refluxed 5 hours and filtered. The solid is extracted with dichloromethane and the extract is washed with 2N citric acid, water and dried (Na2SO4). The solvent is removed in vacuo to give the desired product as a solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05624923 |
| 出典データセット | uspto-grants-1997_04 |
| ORD ID | ord-620dee5a9e52406b8dfbe92ce61103f0 |
| 出典メモ | uspto-grants-1997_04 |