Piperazine → HCID 59758710, compound

HRID 1361103Notes

Reaction equation

HRID 1361103 reaction equation
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.[CH3:7][Si:8]([CH3:23])([CH2:17][CH2:18][Si:19]([CH3:22])([CH3:21])[CH3:20])[CH2:9][CH2:10][CH2:11][O:12][CH2:13][CH:14]1[CH2:16][O:15]1>C(O)C>[CH3:23][Si:8]([CH3:7])([CH2:17][CH2:18][Si:19]([CH3:20])([CH3:22])[CH3:21])[CH2:9][CH2:10][CH2:11][O:12][CH2:13][CH:14]([OH:15])[CH2:16][N:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1

Participants

4

Reactant 2

HCID 4837PiperazineHCID 597587042-{3-[Dimethyl-(2-trimethylsilanyl-ethyl)-silanyl]-propoxymethyl}-oxirane

Product 1

HCID 59758710HCID 59758710, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent3×

Conditions

Temperature
70 °C

Procedure

Piperazine (3.14 g; 36.4 mMol) and 40 mL of ethanol were charged to a 100 mL RB flask equipped with a magnetic stirrer. The mixture was stirred and heated to 70° C. 2-{3-[Dimethyl-(2-trimethylsilanyl-ethyl)-silanyl]-propoxymethyl}-oxirane 8 (2 g; 7.28 mMol) mixed with 10 g ethanol was placed in an addition funnel and added dropwise to the flask. The mixture was stirred and maintained at 70° C. for an additional 4 hours. Ethanol was stripped off on the rotovap. The mixture was distilled under vacuum to remove impurities. Excess piperazine was removed by sublimation.

Workup

  1. customequipped with a magnetic stirrer
  2. customwas placed in an addition funnel
  3. additionadded dropwise to the flask
  4. stirringThe mixture was stirred
  5. temperaturemaintained at 70° C. for an additional 4 hours
  6. distillationThe mixture was distilled under vacuum
  7. customto remove impurities
  8. customExcess piperazine was removed by sublimation

Sources & evidence

ORD record
ord-4d1032a838c040eba310fcedd04caaea
Source dataset
uspto-grants-2011_02
Patent number
US07879916B2

Reaction notes

Loading…