Hydrazine hydrate (1:1) → HCID 66784143, 화합물

온도

80 °C

To a solution of 2,4-dichloro-3-iodopyridine [CAS 343781-36-3] (4.7 g, 17.16 mmol) in 1,4-dioxane (240 ml), was added hydrazine monohydrate (5.096 ml, 102.962 mmol). The reaction mixture was heated in a sealed tube at 80° C. for 16 h. After cooling, the solvent was concentrated in vacuo. The white solid residue thus obtained was dissolved in DCM and washed with NaHCO3 (aqueous saturated solution). The organic layer was separated, dried (Na2SO4) and concentrated in vacuo. The residue was washed with diethylether. The solid thus obtained was discarded. The mothe liquours were concentrated in vacuo to yield intermediate compound D45 (2.31 g, 49%)

1. temperatureAfter cooling
2. concentrationthe solvent was concentrated in vacuo
3. customThe white solid residue thus obtained
4. washwashed with NaHCO3 (aqueous saturated solution)
5. customThe organic layer was separated
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated in vacuo
8. washThe residue was washed with diethylether
9. customThe solid thus obtained
10. concentrationThe mothe liquours were concentrated in vacuo
11. customto yield intermediate compound

ORD 기록

ord-59a1019ffc404e75b8d56339438cf375

출처 데이터셋

uspto-grants-2015_07

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US09085577B2