참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Oxalyl chloride | HCID 65578 | — |
| 반응물 | 2-Amino-4'-methoxyacetophenone | HCID 412889 | — |
| 반응물 | 4-Benzylmorpholine-2-carboxylic acid | HCID 2776353 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | HCID 66990718 | HCID 66990718 | 50.8% |
반응 단계
Oxalyl chloride (2.385 mL, 27.2 mmol) was added to a suspension of 4-(phenylmethyl)-2-morpholinecarboxylic acid (4.02 g, 18.16 mmol) and DMF (0.703 mL, 9.08 mmol) in CH2Cl2 (100 mL) at 0° C. in 10 minutes, and the reaction mixture was stirred at 25° C. for 2 hours. The mixture was concentrated, and the resulting residue was dissolved in CH2Cl2 (100 mL) and triethylamine (5.57 mL, 40.0 mmol). 2-Amino-1-[4-(methyloxy)phenyl]ethanone (3.0 g, 18.16 mmol) was added to the brown solution at 0° C., and the reaction mixture was stirred at 25° C. for 3 hours. Water (150 mL) was added to the reaction mixture, and the aqueous mixture was extracted with EtOAc (3×100 mL). The combined organic layers were dried (Na2SO4), filtered, and evaporated to afford the title compound (3.4 g) as a brown solid. LC-MS (ES) m/z=369 [M+H]+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08697685B2 |
|---|
| 출처 데이터셋 | uspto-grants-2014_04 |
|---|
| ORD ID | ord-972a42a71db94f7792cd6b97db319f32 |
|---|
| 출처 메모 | uspto-grants-2014_04 |
|---|
