Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Diisopropylethylamine → N-Cyclopropyl-N-Methyl-4-{1-[5-Oxo-4-(Tetrahydropyran-4-Ylamino)-6,7-Dihydro-5H-5lambda4-Thieno[3,2-d]Pyrimidin-2-Yl]-Piperidin-4-Yloxy}-Benzamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | (Cyclopropylmethyl)ammonium chloride | HCID 81671 | — |
| 반응물 | Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 9886157 | — |
| 반응물 | 4-{1-[5-oxo-4-(tetrahydropyran-4-ylamino)-6,7-dihydro-5H-5lambda4-thieno[3,2-d]pyrimidin-2-yl]-piperidin-4-yloxy}-benzoic acid | HCID 46912845 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | N-Cyclopropyl-N-Methyl-4-{1-[5-Oxo-4-(Tetrahydropyran-4-Ylamino)-6,7-Dihydro-5H-5lambda4-Thieno[3,2-d]Pyrimidin-2-Yl]-Piperidin-4-Yloxy}-Benzamide | HCID 46913023 | — |
반응 단계
55 mg of Example 184 (see 40.) are placed in 2 ml dimethylformamide, then 81 l diisopropylethylamine and 53.1 mg O-(7-azabenzotriazol-1-yl-)-N,N,N′,N′-tetramethyluronium hexafluorophosphate (HATU) are added. After 15 min 13.8 mg cyclopropylmethylamine hydrochloride are added. The reaction mixture is stirred at ambient temperature until there is no further reaction and the product is purified directly by preparative HPLC (method B). 30 mg of Example 242 are obtained as a solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08754073B2 |
| 출처 데이터셋 | uspto-grants-2014_06 |
| ORD ID | ord-f5998a79fbcc4c73bfae8095fdc14141 |
| 출처 메모 | uspto-grants-2014_06 |