Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium hydride → 5-Cyclopentyloxy-1-(3,5-dichloropyridin-4-ylmethyl)-6-methoxy-phthalazine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 3,5-Dichloro-4-methylpyridine | HCID 10953827 | — |
| 반응물 | 1-Chloro-5-cyclopentyloxy-6-methoxy-phthalazine | HCID 11821961 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 5-Cyclopentyloxy-1-(3,5-dichloropyridin-4-ylmethyl)-6-methoxy-phthalazine | HCID 9865916 | 57.1% |
반응 단계
Under stirring, 55% sodium hydride (3.73 g, 85.56 mmoles) was added to a solution, under nitrogen, of 3,5-dichloro-4-methyl-pyridine (13.86 g, 85.56 mmoles) in anhydrous DMF (100 ml). The mixture was kept under stirring for 1 hour then added with a solution of 1-chloro-5-cyclopentyloxy-6-methoxy-phthalazine (7.95 g, 28.52 mmoles), obtained as described in example 7, in anhydrous dimethylformamide (70 ml). After resting overnight, the mixture was quenched with water, diluted with water and extracted with ethyl acetate. The extract was washed with water and dried on sodium sulphate, then evaporated to dryness. The residue was flash chromatographed (eluent petrolatum/ethyl acetate 1:1) to give 6.58 g of the title compound (yield: 57%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06340684B1 |
| 출처 데이터셋 | uspto-grants-2002_01 |
| ORD ID | ord-00569ee8d4b944d9b7cff0b9d89c3f73 |
| 출처 메모 | uspto-grants-2002_01 |