Hydrazine hydrate (1:1) → HCID 66784143、化合物

温度

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レコード

ord-5dc878b77b224ef0a6832c65de900c8e

出典データセット

uspto-grants-2014_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08716480B2