참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Morpholine | HCID 8083 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 3-Nitrobenzoic acid | HCID 8497 | — |
| 반응물 | Oxalyl chloride | HCID 65578 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | Morpholino(3-nitrophenyl)methanone | HCID 225453 | 69.4% |
반응 단계
To stirred solution of 3-nitrobenzoic acid (5 g, 29.9 mmol) in DCM: DMF (30 ml, 29:1) was added oxalyl chloride (3.14 ml, 35.9 mmol) dropwise at RT. Resulting reaction mixture was stirred for 1 h. The mixture was concentrated and the residue was dissolved in DCM (25 ml), the reaction mixture was cooled to 0° C. and triethylamine (6.26 ml, 44.9 mmol) and morpholine (3.13 ml, 35.9 mmol) were added and the reaction mixture was stirred for 1 h. The reaction mixture was concentrated under vacuum and the residue was diluted with cold water, the solid separated out was filtered and washed with n-hexanes and dried under vacuum to give the product (4.9 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US09428499B2 |
|---|
| 출처 데이터셋 | uspto-grants-2016_08 |
|---|
| ORD ID | ord-2ceddaf9a6db4f9eb02bae758ec6561c |
|---|
| 출처 메모 | uspto-grants-2016_08 |
|---|