反応 #1265389

ord-31c589ad82a64b609705114404987e8b

反応方程式

COC(C)(OC)c1ncc(Cl)s1
5-Chloro-2-(1,1-dimethoxy-ethyl)-thiazole
O=C(O)C(F)(F)F
trifluoroacetic acid
O
water
CC(=O)c1ncc(Cl)s1
sub-titled compound
CC(=O)c1ncc(Cl)s1
1-(5-Chloro-thiazol-2-yl)-ethanone

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    濃縮concentrated to an oil
  2. 2
    workup.ADDITIONdiluted with diethyl ether
  3. 3
    洗浄washed with 10% sodium bicarbonate, water and brine
  4. 4
    乾燥dried (magnesium sulfate)
  5. 5
    ろ過filtered
  6. 6
    濃縮concentrated

実験手順

To a solution of 5-Chloro-2-(1,1-dimethoxy-ethyl)-thiazole (3.5 g) in dichloromethane (20 ml) was added trifluoroacetic acid (30 ml) and water (1 ml). The resulting mixture was stirred overnight at ambient, concentrated to an oil, diluted with diethyl ether, washed with 10% sodium bicarbonate, water and brine, dried (magnesium sulfate), filtered and concentrated to afford the sub-titled compound as a yellow solid in quantitative yield (2.6 g); 1H NMR (400 Mhz, CDCl3) δ 2.7 (3H, s), 7.8 (1H, s).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07276502B2uspto-grants-2007_10