反応 #1755475

ord-faaabf0ccac44fbb9b9eb6a8c2b262c3

反応方程式

C#CCN1CCN(C(=O)OC(C)(C)C)CC1
4-Prop-2-ynyl-piperazine-1-carboxylic acid tert-butyl ester
O=C(O)C(F)(F)F
TFA
C#CCN1CCNCC1
product
C#CCN1CCNCC1
1-Prop-2-ynyl-piperazine

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他bubbled
  2. 2
    workup.ADDITIONThe additional portions of TFA were added when this activity
  3. 3
    workup.ADDITIONAfter the third portion of TFA had been added only minimal
  4. 4
    その他bubbling
  5. 5
    その他evaporated under reduced pressure

実験手順

To a flame-dried 25 mL round bottom flask under nitrogen was added 2.1 g of 4-Prop-2-ynyl-piperazine-1-carboxylic acid tert-butyl ester. To this solid was added 5 mL of 98% TFA in 1 mL portions. The solution turned wine red, bubbled and smoked. The additional portions of TFA were added when this activity subsided. After the third portion of TFA had been added only minimal bubbling occurred. The solution was allowed to stir under nitrogen at room temperature for an additional hour and evaporated under reduced pressure to yield the product as a thick red syrup. Assumed quantitative yield of 1.16 g. The residue was suspended in 20 mL dichloromethane and used immediately without further purification for the preparation of compounds JR4031, JR4033, and JR4035.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07989431B2uspto-grants-2011_08