反応 #9272

ord-7e0ae6c8d873495eb76902d9b21f0789

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The solvent was removed under reduced pressure
  2. 2
    その他the crude reaction mixture
  3. 3
    その他was purified by preparative HPLC
  4. 4
    その他LC/MS 2.86 min, 341 (M+1)

実験手順

About 0.2 g of 2-[(ethylamino)Carbonyl]amino-1,3-benzothiazole-6-carboxylic acid was dissolved into about 20 mL dichloromethane and about 0.2 mL triethylamine. Added about 1 eq of the appropriate amine followed by about 0.3 g of 1-ethyl-3-(3-dimethylaminopropyl)Carbodiimide hydrochloride then stirred at room temperature for about 12–24 hours. The solvent was removed under reduced pressure then the crude reaction mixture was purified by preparative HPLC. 1H NMR 1.10 (t, 3H), 3.2 (m, 2H), 6.76 (br s, 11), 7.10 (m, 1H), 7.36 (m, 2H), 7.70 (d, 1H), 7.79 (d, 2H), 7.97 (m, 1H), 8.5 (s, 1H), 10.23 (s, 1H), 10.9 (br s, 1H); LC/MS 2.86 min, 341 (M+1);

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07091227B2uspto-grants-2006_08