反応 #90240

ord-820bf830bd7040b0b9ca890ad376d2e0

反応方程式

O=C(Cl)C(=O)Cl
oxalyl chloride
CN(C)C=O
dimethylformamide
O=C(O)c1c[nH]c2ccccc12
indole-3-carboxylic acid
O=C(Cl)C(=O)Cl
oxalyl chloride
O=C(Cl)c1c[nH]c2ccccc12
indole-3-carbonyl chloride

溶媒

反応条件

温度
23°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他producing a clear, slightly yellow solution
  2. 2
    その他This solution was evaporated to dryness in vacuo at 0.1 Torr
  3. 3
    その他removal of excess oxalyl chloride
  4. 4
    workup.DISSOLUTIONwas subsequently re-dissolved in 2 ml of dry DCM

実験手順

Next, a solution of indole-3-carbonyl chloride was prepared. A well-stirred suspension of indole-3-carboxylic acid (67.7 mg, 0.42 mmol) in dry DCM (2 ml) containing a small amount of dimethylformamide (DMF) (20 μL) was treated with oxalyl chloride (0.84 mmol, 107 mg, 72 μL) at 0° C. Following addition to the oxalyl chloride, the mixture was stirred for 20 minutes at 23° C., producing a clear, slightly yellow solution. This solution was evaporated to dryness in vacuo at 0.1 Torr to ensure removal of excess oxalyl chloride, and was subsequently re-dissolved in 2 ml of dry DCM.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09445596B2uspto-grants-2016_09