Реакция #167332

Уравнение реакции

Hydrazine hydrate

2-fluoro-5-[3-(4-methyl-pyridin-3-yl)-2-oxo-imidazolidin-1-yl]-benzonitrile

2-Fluoro-5-[3-(4-methyl-pyridin-3-yl)-2-oxo-imidazolidin-1-yl]-benzonitrile

MeOH

→

product

Выход 45.3%

1-(3-Amino-1H-indazol-5-yl)-3-(4-methyl-pyridin-3-yl)-imidazolidin-2-one

Выход 45.3%

Растворители

—

2-methoxymethanol

CHCl3

Условия реакции

Обработка

1. 1
   Температураmaintained for 20 hours
2. 2
   ДругоеThe reaction mixture was partitioned between ice water and DCM
3. 3
   СушкаThe organic layer was dried over Na2SO4
4. 4
   Концентрированиеconcentrated
5. 5
   ДругоеPurification by column chromatography on silica gel (10% MeOH in CHCl3)

Методика

Hydrazine hydrate (5 mL) was added to solution of 2-fluoro-5-[3-(4-methyl-pyridin-3-yl)-2-oxo-imidazolidin-1-yl]-benzonitrile (103A: 265 mg) in 2-methoxymethanol (5 mL). The resulting mixture was heated to 170° C. and maintained for 20 hours. The reaction was monitored by TLC (20% MeOH in CHCl3). The reaction mixture was partitioned between ice water and DCM. The organic layer was dried over Na2SO4 and concentrated. Purification by column chromatography on silica gel (10% MeOH in CHCl3) afforded 125 mg of the product (45.3% yield).

Источник