تفاعل #1702116
ord-003dbe4c8da8459f95df39b55fd09568
معادلة التفاعل
N-(3-aminobenzyl)-2,5-dichloropyrimidin-4-amine
hydrogen chloride
triethylamine
m-nitrobenzenesulfonyl chloride
→
desired product
المردود 95.0%
N-(3-{[(2,5-Dichloropyrimidin-4-yl)amino]methyl}phenyl)-3-nitrobenzenesulfonamide
المردود 95.0%
المتفاعلات
الكواشف
لا شيء
المذيبات
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1أخرىthe solvent was removed under vacuum
- 2workup.ADDITIONThe residue was treated with EtOAc and water
- 3تجفيفThe organic layer was dried over Na2SO4
- 4ترشيحfiltered
- 5تركيزconcentrated under vacuum
الإجراء التجريبي
To a mixture of N-(3-aminobenzyl)-2,5-dichloropyrimidin-4-amine.hydrogen chloride (0.20 g, 0.58 mmol) and triethylamine (0.32 mL, 2.3 mmol) in THF (3 mL) was added slowly m-nitrobenzenesulfonyl chloride (0.13 g, 0.58 mmol). The resulting mixture was stirred at rt for 2 hours and the solvent was removed under vacuum. The residue was treated with EtOAc and water. The organic layer was dried over Na2SO4, filtered, and concentrated under vacuum to provide the desired product (0.30 g, 95%). LCMS for C17H14Cl2N5O4S (M+H)+: m/z=453.9, 455.9.