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Methanol → 4-(9-Thia-1,5,7-triaza-fluoren-8-yl)-piperazine-1-carbothioic acid [4-(Pyrimidin-2-ylsulfamoyl)-phenyl]-amide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | 4-Piperazinopyrido[3',2';4,5]thieno[3,2-d]pyrimidine | HCID 67390286 | — |
| 反応物 | N-Pyrimidin-2-yl-4-thioformylamino-benzenesulfonamide chloride | HCID 86601004 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-(9-Thia-1,5,7-triaza-fluoren-8-yl)-piperazine-1-carbothioic acid [4-(Pyrimidin-2-ylsulfamoyl)-phenyl]-amide | HCID 59020502 | — |
反応手順
To a solution of 4-piperazinopyrido[3′,2′;4,5]thieno[3,2-d]pyrimidine (200 mg, 0.74 mmol) and pyridine (0.5 mL, 7.9 mmol) in dichloromethane (20 mL) was added a solution of product 1d in dichloromethane (20 mL) and this was stirred overnight. Methanol was added to quench excess thiophosgene, and the residue after removal of solvent was purified by silica gel column chromatography eluting with 5% methanol/dichloromethane and further recrystallized from dichloromethane/hexane to give 60 mg (15%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08999988B2 |
| 出典データセット | uspto-grants-2015_04 |
| ORD ID | ord-5c1a14dc95934e17a86498fea3f62005 |
| 出典メモ | uspto-grants-2015_04 |