Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methanol → 4-(9-Thia-1,5,7-triaza-fluoren-8-yl)-piperazine-1-carbothioic acid [4-(Pyrimidin-2-ylsulfamoyl)-phenyl]-amide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | Pyridine | HCID 1049 | — |
| 반응물 | 4-Piperazinopyrido[3',2';4,5]thieno[3,2-d]pyrimidine | HCID 67390286 | — |
| 반응물 | N-Pyrimidin-2-yl-4-thioformylamino-benzenesulfonamide chloride | HCID 86601004 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 4-(9-Thia-1,5,7-triaza-fluoren-8-yl)-piperazine-1-carbothioic acid [4-(Pyrimidin-2-ylsulfamoyl)-phenyl]-amide | HCID 59020502 | — |
반응 단계
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%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07326713B2 |
| 출처 데이터셋 | uspto-grants-2008_02 |
| ORD ID | ord-79b7308711f64f608b638a44c50dd5c2 |
| 출처 메모 | uspto-grants-2008_02 |