Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Diisopropylethylamine → HCID 44561082, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 4-(Methylamino)tetrahydro-2H-pyran | HCID 6991950 | — |
| 반응물 | ethyl 4-chloro-1-ethyl-1H-pyrazolo[3,4-b]pyridine-5-carboxylate | HCID 10491120 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | HCID 44561082 | HCID 44561082 | 76.5% |
반응 단계
Intermediate 1 (1.2 g, 4.76 mmol), Intermediate 50 (0.79 g, 5.2 mmol) and diisopropylethylamine (4 ml, 24 mmol) in MeCN (8 ml) was heated at 70° C. for 24 hours. The solvent was removed in vacuo and the residue partitioned between DCM and water. The organic phase was concentrated in vacuo and the residue chromatographed on silica (50 g) eluting with cyclohexane:ethyl acetate (2:1 followed by 1:1 then 1:2). Appropriate fractions were combined and evaporated to give Intermediate 51 as a brown oil (1.21 g). LCMS showed MH+=334; TRET=2.61 min.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07528148B2 |
| 출처 데이터셋 | uspto-grants-2009_05 |
| ORD ID | ord-6bb30160f5c549bca1f5b8d0dc14c418 |
| 출처 메모 | uspto-grants-2009_05 |