Ammonium Hydroxide → HCID 57459596, compound

Temperature

70 °C

To a solution of compound D1 (8 g, 29.21 mmol) in 1,4-dioxane (450 ml), was added hydrazine monohydrate (14.169 ml, 175.255 mmol). The reaction mixture was heated in a sealed tube at 70° C. for 16 h. After cooling, NH4OH (32% aqueous solution) was added and the resulting mixture was concentrated in vacuo. The white solid residue thus obtained was taken up in EtOH to obtain a suspension which was heated and filtered. The filtrate was cooled and the precipitate thus obtained was filtered off. The resulting filtrate was concentrated in vacuo to yield intermediate compound D2 (2.67 g, 52%) as a white solid.

1. temperatureAfter cooling
2. concentrationthe resulting mixture was concentrated in vacuo
3. customThe white solid residue thus obtained
4. customto obtain a suspension which
5. temperaturewas heated
6. filtrationfiltered
7. temperatureThe filtrate was cooled
8. customthe precipitate thus obtained
9. filtrationwas filtered off
10. concentrationThe resulting filtrate was concentrated in vacuo

ORD record

ord-bb9d9ff83c0e458d9457ef5baee3af52

Source dataset

uspto-grants-2015_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08946205B2