反応 #82198

ord-5719a89c5ebc469f95c58c4d87481c91

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    濃縮concentrated in vacuo
  2. 2
    乾燥dried over Na2SO4
  3. 3
    濃縮concentrated in vacuo
  4. 4
    その他Purification of the residue by silica gel chromatography

実験手順

A solution of 40 g of 4-(chloromethyl)-2-isopropylthiazole hydrochloride in 100 ml of water was added dropwise with stirring to 400 ml of 40% aqueous methylamine. The resulting solution was stirred for 1 h, then concentrated in vacuo. The residue was taken up in chloroform, dried over Na2SO4, and concentrated in vacuo. Purification of the residue by silica gel chromatography using 10% methanol in chloroform provided 21.35 g (55%) of the desired compound. 1H NMR (DMSO-d6) δ 1.34 (d, J=7 Hz, 6 H), 2.56 (s, 3 H), 3.30 (heptet, J=7 Hz, 1 H), 4.16 (s, 2 H), 7.63 (s, 1 H). Mass spectrum: (M+H)+ =171.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05621109uspto-grants-1997_04