Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Piperazine | HCID 4837 | — |
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Triisopropylsilyl chloride | HCID 139400 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | HCID 131734484 | HCID 131734484 | — |
Reaction Steps
A flask equipped with a stirrer, reflux condenser, dropping funnel and thermometer was charged with 189.4 g (2.2 mol) of piperazine, 200 ml of xylene, and 1.0 g (0.01 mol) of methanesulfonic acid and heated at 130° C. Once the internal temperature became steady, 192.8 g (1.0 mol) of triisopropylchlorosilane was added dropwise over 2 hours. Stirring was continued for 10 hours at the temperature. The reaction solution was cooled to room temperature, to which 500 g of a 10 wt % sodium hydroxide aqueous solution was added. The organic layer was separated. On distillation, 132.6 g of a fraction having a boiling point of 109-111° C./0.4 kPa was collected, which was 1-triisopropylsilylpiperazine.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09233988B2 |
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| Source dataset | uspto-grants-2016_01 |
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| ORD ID | ord-68d58d72e3924fb5bfe816ca2db0a603 |
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| Source note | uspto-grants-2016_01 |
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