反応 #9184

ord-8e2c9bc4dca442bda6037a7be6b1f8b6

反応条件

温度
55°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The solution was cooled to 0° C.
  2. 2
    その他The solvent was evaporated in vacuo
  3. 3
    洗浄The residue was washed with water, diethyl ether
  4. 4
    乾燥dried in vacuo over anhydrous phosphorous pentoxide
  5. 5
    その他to obtain the title acid (6 g, 89%) as a white solid

実験手順

A stirred solution of ethyl-2-tert-butoxycarbonyloxyamino-4-methyl-thiazole-5-carboxylate (10 g, 34.95 mmol) in tetrahydrofuran-ethanol (250 mL, 2:3) was treated with a 6N KOH solution (250 mL). The mixture was heated to 55° C. overnight. The solution was cooled to 0° C. and acidified with concd. HCl to pH 1. The solvent was evaporated in vacuo. The residue was washed with water, diethyl ether, dried in vacuo over anhydrous phosphorous pentoxide to obtain the title acid (6 g, 89%) as a white solid.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07091223B2uspto-grants-2006_08