反応 #1365707

ord-63934e57f4b2442c9adff995dd7c839f

反応条件

温度
25°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他fitted with agitator
  2. 2
    workup.ADDITIONthermocouple, nitrogen inlet and addition funnel with condenser
  3. 3
    温度The reactor was maintained at 25° C. for an additional 5 hours at which time the product
  4. 4
    workup.ADDITIONwas poured into glass containers
  5. 5
    その他sealed under a blanket of nitrogen
  6. 6
    workup.WAITAfter one week the unsaturation number was
  7. 7
    その他at 25° C.

実験手順

1482 parts (8.27 equiv.) of 3-aminopropyltrimethoxysilane were added to a 5 liter flask fitted with agitator, thermocouple, nitrogen inlet and addition funnel with condenser. 1423.2 parts (8.27 equiv.) of diethyl maleate were added dropwise through the addition funnel over a period of 2 hours. The temperature of the reactor was maintained at 25° C. during the addition. The reactor was maintained at 25° C. for an additional 5 hours at which time the product was poured into glass containers and sealed under a blanket of nitrogen. After one week the unsaturation number was 0.6 indicating the reaction was ˜99% complete. The product, N-(3-trimethoxysilyipropyl) aspartic acid diethyl ester, had a viscosity of 11 mPa.s at 25° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06444325B1uspto-grants-2002_09