Piperazine → HCID 67062407, compound

HRID 602236

Reaction equation

HRID 602236 reaction equation
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.ClC[Si:9]([O:16][CH2:17][CH3:18])([O:13][CH2:14][CH3:15])[O:10][CH2:11][CH3:12].[SiH4].Cl.N1CCNC[CH2:22]1>C1(C)C(C)=CC=CC=1>[CH2:14]([O:13][Si:9]([O:16][CH2:17][CH3:18])([O:10][CH2:11][CH3:12])[N:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH:2]1[CH3:22])[CH3:15]

Participants

6

Reactant 4

HCID 4837Piperazine2×HCID 23953SilaneHCID 82044Piperazine, hydrochloride (1:?)HCID 84858Silane, (chloromethyl)triethoxy-

Product 1

HCID 67062407HCID 67062407, compound

Reagents, catalysts & solvents 1

HCID 7237O-XyleneSolvent

Conditions

Temperature
110 °C

Procedure

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.

Workup

  1. dissolutiondissolves completely
  2. additionAdded dropwise at this temperature
  3. customover the course of 1 h
  4. customis precipitated as a salt
  5. customthe suspension remains readily stirrable until the end of the reaction
  6. additionAfter the end of the addition
  7. filtrationthe precipitated salt is filtered off on a preheated filter

Sources & evidence

ORD record
ord-045ff6c78d274fb1a672d1d1591d8ae4
Source dataset
uspto-grants-2011_03
Patent number
US07906179B2

Linked notes

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