Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Piperazine | HCID 4837 | — |
| Reactant | Silane | HCID 23953 | — |
| Reactant | Piperazine, hydrochloride (1:?) | HCID 82044 | — |
| Reactant | Silane, (chloromethyl)triethoxy- | HCID 84858 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | HCID 67062407 | HCID 67062407 | — |
Reaction Steps
905.3 g (10.5 mol) of piperazine and 945 ml of xylene (anhydrous) as solvent are charged to a 4 liter 4-neck flask and subsequently innertized with nitrogen. The batch is heated to a temperature of 100° C., in the course of which the piperazine dissolves completely. Added dropwise at this temperature are 446.3 g (2.1 mol) of chloromethyltriethoxysilane, over the course of 1 h with thorough stirring. Following the addition of about ⅓ of the amount of silane, piperazine hydrochloride is precipitated as a salt, but the suspension remains readily stirrable until the end of the reaction. After the end of the addition, stirring is continued for a further 15 min. Subsequently the reaction mixture is heated to 110° C. and the precipitated salt is filtered off on a preheated filter.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07906179B2 |
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| Source dataset | uspto-grants-2011_03 |
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| ORD ID | ord-045ff6c78d274fb1a672d1d1591d8ae4 |
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| Source note | uspto-grants-2011_03 |
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