Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1-Naphthalenemethanol → 6-Chloro-2-(1-naphthylmethoxy)pyrimidin-4-amine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1-Naphthalenemethanol | HCID 20908 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 4-Pyrimidinamine, 2,6-dichloro- | HCID 82387 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 6-Chloro-2-(1-naphthylmethoxy)pyrimidin-4-amine | HCID 470508 | — |
반응 단계
1-Naphthalenemethanol (227 mg, 1.44 mmol) is added to a slurry of 50% sodium hydride (69 mg, 1.44 mmol) in dry THF (4 ml) at 0° C. After stirring for 30 minutes, 4-amino-2,6-dichloropyrimidine (157 mg, 0.96 mmol) is added and stirred at 22° C. for 72 hours. The solution is quenched with saturated NH4Cl and concentrated in vacuo. The residue is dissolved in methylene chloride and washed 3× saturated NaHCO3, dried with MgSO4, filtered, and concentrated in vacuo. The sample is purified by chromatography using 1:2 ethyl acetate/hexanes and recrystallization from heptane/toluene, mp 160-161° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05981537 |
| 출처 데이터셋 | uspto-grants-1999_11 |
| ORD ID | ord-fb5c01d00e954664a2426336b92669f7 |
| 출처 메모 | uspto-grants-1999_11 |