Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triphenylphosphine → 1,1-dimethylethyl 4-(5-bromo-4-chloro-7H-pyrrolo[2,3-d]pyrimidin-7-yl)-1-piperidinecarboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | Tert-butyl 4-hydroxypiperidine-1-carboxylate | HCID 643502 | — |
| 반응물 | Diethyl azodicarboxylate | HCID 5462977 | — |
| 반응물 | HCID 178478408 | HCID 178478408 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 1,1-dimethylethyl 4-(5-bromo-4-chloro-7H-pyrrolo[2,3-d]pyrimidin-7-yl)-1-piperidinecarboxylate | HCID 58057890 | 86.2% |
반응 단계
To a solution of 5-bromo-4-chloro-1H-pyrrolo[2,3-d]pyrimidine (214 mg, 0.921 mmol), 1,1-dimethylethyl 4-hydroxy-1-piperidinecarboxylate (556 mg, 2.76 mmol) and triphenylphosphine (483 mg, 1.841 mmol) in Tetrahydrofuran (THF) (10 mL) was added by drop wise DEAD (0.291 mL, 1.841 mmol). The solution was let stir at room temp. After 2 hr the reaction was concentrated and purified by silica gel chromatography to afford 1,1-dimethylethyl 4-(5-bromo-4-chloro-7H-pyrrolo[2,3-d]pyrimidin-7-yl)-1-piperidinecarboxylate (330 mg, 86% yield) as a white solid
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08598156B2 |
| 출처 데이터셋 | uspto-grants-2013_12 |
| ORD ID | ord-52c7bacafd3440db8edef2af04291fd4 |
| 출처 메모 | uspto-grants-2013_12 |