반응 #802285

반응 방정식

tert-butyl (5-(7-chloro-2-methyl-1,6-naphthyridin-3-yl)-2,4-difluorophenyl)carbamate

XantPhos

Cs2CO3

acetamide

→

title compound

수율 90.0%

tert-butyl (5-(7-acetamido-2-methyl-1,6-naphthyridin-3-yl)-2,4-difluorophenyl)carbamate

수율 90.0%

용매

dioxane

반응 조건

후처리

1. 1
   기타Sparge
2. 2
   온도Cool to RT
3. 3
   기타remove the solids
4. 4
   여과via filtration through diatomaceous earth
5. 5
   세척rinse well with THF
6. 6
   농축concentrate the filtrate to dryness
7. 7
   기타purify via silica gel chromatography (EtOAc/Hex)

실험 절차

Sparge a mixture of tert-butyl (5-(7-chloro-2-methyl-1,6-naphthyridin-3-yl)-2,4-difluorophenyl)carbamate (0.664 g, 1.636 mmol), XantPhos (0.189 g, 0.327 mmol), Cs2CO3 (1.066 g, 3.27 mmol) and acetamide (0.483 g, 8.18 mmol) in dioxane (16 mL) with Ar, add Pd2(dba)3 (0.150 g, 0.164 mmol) and heat at 100° C. overnight. Cool to RT, remove the solids via filtration through diatomaceous earth, rinse well with THF, concentrate the filtrate to dryness and purify via silica gel chromatography (EtOAc/Hex) to afford the title compound (630 mg, 90%) as a glass. MS (ESI) m/z: 429.2 (M+H+).

출처