Реакция #547117

Уравнение реакции

mixture

7-(R)-(4-Fluoro-2-methyl-phenyl)-[1,4]-diazepane-1-carboxylic acid, (3,5-dichloro-benzyl)-methylamide hydrochloride

formaldehyde

sodium triacetoxyacetoxyborohydride

→

7-(R)-(4-fluoro-2-methyl-phenyl)-4-methyl-[1,4]-diazepane-1-carboxylic acid, (3,5-dichloro-benzyl)-methylamide

Выход 20.6%

Растворители

1,2-dichloroethane

Условия реакции

Обработка

1. 1
   ПромывкаThe mixture was washed with water (2 mL) and brine (2 mL)
2. 2
   Концентрированиеconcentrated in vacuo
3. 3
   ДругоеThe residue was purified by flash chromatography (AcOEt 100%)

Методика

A mixture of example 6 (51 mg), aqueous formaldehyde (33 μL) and sodium triacetoxyacetoxyborohydride (50 mg) in anhydrous 1,2-dichloroethane (2 mL) was stirred at r.t. overnight. The mixture was washed with water (2 mL) and brine (2 mL) and concentrated in vacuo. The residue was purified by flash chromatography (AcOEt 100%) to give 7-(R)-(4-fluoro-2-methyl-phenyl)-4-methyl-[1,4]-diazepane-1-carboxylic acid, (3,5-dichloro-benzyl)-methylamide (10 mg).

Источник