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 Et2O. The solid thus obtained was discarded. The mother liquours were concentrated in vacuo to yield intermediate compound D32 (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 Et2O
9. customThe solid thus obtained
10. concentrationThe mother liquours were concentrated in vacuo
11. customto yield intermediate compound D32 (2.31 g, 49%)

ORDレコード

ord-17b56f207eac483f93e75b4f4e77a5ef

出典データセット

uspto-grants-2015_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08946205B2