반응 #9216
ord-1a6875afea914c3fb284eeb3add847f4
반응 방정식
반응 조건
온도
100°CELSIUS
상세 조건
See reaction.notes.procedure_details.
후처리
- 1기타was bubbled with nitrogen gas for 5 minutes
- 2온도The mixture was cooled down
- 3기타evaporated to dryness
- 4기타Purification by flash chromatography on SiO2 with ethyl acetate and heptane (2/1)
실험 절차
A mixture of 1-(7-trifluoromethylsulfonyl-2-benzothiazolyl)-3-ethylurea (0.080 g, 80% pure, 0.17 mmol), Pd(PPh3)2Cl2 (0.010 g, 0.014 mmol, 0.08 eq), and triethylamine (0.102 mL, 0.73 mmol, 4.3 eq) in 1 mL of anhydrous DMF was bubbled with nitrogen gas for 5 minutes, followed by the addition of trimethylsilyl acetylene (0.12 mL, 0.85 mmol, 5.0 eq). The mixture was heated at about 100° C. with stirring in a sealed tube for about 18 hours. The mixture was cooled down, taken up in 10 mL MeOH, and evaporated to dryness. Purification by flash chromatography on SiO2 with ethyl acetate and heptane (2/1) gave pure desired compound 0.050 g (93%). LC/MS 318 (M+1); LC retention time 9.25 min.