Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1,2-Dichloroethane → (4-Isopropyl-piperazin-1-yl)-[6-(2-piperidin-1-yl-ethylamino)-pyridin-3-yl]-methanone
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1,2-Dichloroethane | HCID 11 | — |
| 반응물 | 4-Methylmorpholine | HCID 7972 | — |
| 반응물 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 반응물 | 1-Isopropylpiperazine | HCID 78013 | — |
| 반응물 | 6-Chloronicotinic acid | HCID 79222 | — |
| 반응물 | (6-Chloro-pyridin-3-yl)-(4-isopropyl-piperazin-1-yl)-methanone | HCID 43420904 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | Sodium Hydroxide | HCID 14798 | — |
| 생성물 | Ammonia | HCID 222 | 2% |
| 생성물 | (4-Isopropyl-piperazin-1-yl)-[6-(2-piperidin-1-yl-ethylamino)-pyridin-3-yl]-methanone | HCID 11710212 | 56% |
반응 단계
(6-Chloro-pyridin-3-yl)-(4-isopropyl-piperazin-1-yl)-methanone. To a solution of 6-chloronicotinic acid (0.985 g, 6.25 mmol) and 1-isopropyl-piperazine (1.50 g, 7.50 mmol) in DCM (100 mL) was added HOBt (1.20 g, 9.40 mmol), EDC (1.80 g, 9.40 mmol), and N-methyl morpholine (3.4 mL, 31.3 mmol). After 18 h the reaction was diluted with 1 N NaOH (50 mL) and extracted with DCM (3×50 mL). The organic extracts were combined, dried (Na2SO4), and concentrated. Chromatography of the residue (SiO2: 2-4% 2 M NH3 in MeOH/DCM) gave the title compound as a solid (0.934 g, 56%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07947718B2 |
| 출처 데이터셋 | uspto-grants-2011_05 |
| ORD ID | ord-f19ecca019454a139282c3ef390b44e3 |
| 출처 메모 | uspto-grants-2011_05 |