참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 6-fluoro-2-(4-methoxybenzyl)-7-methylisoquinolin-1(2H)-one | HCID 59226043 | — |
| 반응물 | HCID 178479278 | HCID 178479278 | — |
| 용매 | Dimethylacetamide | HCID 31374 | — |
| 생성물 | HCID 178490766 | HCID 178490766 | — |
반응 단계
To a solution of 1.48 g (9.75 mmol) of trans-4-aminocyclohexanol hydrochloride in 20 ml of dimethylacetamide were added 1.95 g (48.77 mmol) of sodium hydride (60%) and the mixture was stirred for 15 minutes. Subsequently 2.90 g (9.75 mmol) of 6-fluoro-2-(4-methoxy-benzyl)-7-methyl-2H-isoquinolin-1-one in 30 ml of dimethylacetamide were added and the reaction mixture was heated to 80° C. for 2 days. After cooling, the mixture was poured into 300 ml of ice water and the precipitated crude product was purified by chromatography. First the remaining starting material was eluted with ethyl acetate/heptane (2:1) and finally the desired product was eluted by pure methanol giving 1.98 g 6-(trans-4-amino-cyclohexyloxy)-2-(4-methoxy-benzyl)-7-methyl-2H-isoquinolin-1-one.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08742116B2 |
|---|
| 출처 데이터셋 | uspto-grants-2014_06 |
|---|
| ORD ID | ord-6a42facfdc81435ba4a6b2d4ddd95035 |
|---|
| 출처 메모 | uspto-grants-2014_06 |
|---|