反応 #43813

ord-f6128a8659ec446c9f3f2996b643353f

溶媒

反応条件

温度
110°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    濃縮The reaction was concentrated to dryness
  2. 2
    workup.DISSOLUTIONredissolved in toluene (2 mL)
  3. 3
    温度the reaction was heated overnight
  4. 4
    その他reaction
  5. 5
    濃縮The reaction was then concentrated

実験手順

The product of step b.) (33 mg, 0.069 mmol) was stirred in methanol (2 mL) with Et3N (10 μL, 0.069 mmol) at 65° C. for two hours without change. The reaction was concentrated to dryness and redissolved in toluene (2 mL). Et3N (10 μL, 0.069 mmol) was added to the solution and the reaction was heated to 110° C. overnight. Additional Et3N (35 μL, 0.242 mmol) was added and the reaction was heated overnight to complete reaction. The reaction was then concentrated to give the sub-title compound that was used in crude form without purification. MS: ESI (positive): 456 (M+H).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07732618B2uspto-grants-2010_06