Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Diisopropylethylamine → tert-butyl-N-[1-oxo-1-[[1-(2-thiophen-3-ylethynyl)isoquinolin-3-yl]amino]-propan-2-yl]carbamate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 3-Ethynylthiophene | HCID 3548422 | — |
| 반응물 | tert-butyl-N-[1-[(1-bromoisoquinolin-3-yl)amino]-1-oxopropan-2-yl]carbamate | HCID 86694369 | — |
| 촉매 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 촉매 | HCID 178418476 | HCID 178418476 | — |
| 용매 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 생성물 | tert-butyl-N-[1-oxo-1-[[1-(2-thiophen-3-ylethynyl)isoquinolin-3-yl]amino]-propan-2-yl]carbamate | HCID 86694425 | — |
반응 단계
A mixture of tert-butyl-N-[1-[(1-bromoisoquinolin-3-yl)amino]-1-oxopropan-2-yl]-carbamate B4a (150 mg, 0.38 mmol), 3-ethynylthiophene (45 mg, 0.42 mmol), copper(I) iodide (7 mg, 0.04 mmol), Dichlorobis(triphenylphosphine)palladium(II) (27 mg, 0.04 mmol) and DIPEA (200 μl, 2 mmol) is stirred under argon atmosphere in NMP (1 ml) for 1 h at 80° C. The mixture is concentrated in vacuo and the product purified by RP HPLC. Yield: 102 mg (64%). HPLC-MS: M+H=422; tR=1.99 min (*Method—4).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08859541B2 |
| 출처 데이터셋 | uspto-grants-2014_10 |
| ORD ID | ord-213eef32a6e54583a136012b6b2cad62 |
| 출처 메모 | uspto-grants-2014_10 |