n-Butyl allophanate → Dibutyl carbonate

HRID 278526Notes

Reaction equation

HRID 278526 reaction equation
[C:1]([O:7][CH2:8][CH2:9][CH2:10][CH3:11])(=[O:6])NC(N)=O>C(O)CCC>[C:1](=[O:6])([O:7][CH2:8][CH2:9][CH2:10][CH3:11])[O:7][CH2:8][CH2:9][CH2:10][CH3:11]

Participants

3

Reactant 1

HCID 5315565n-Butyl allophanate

Product 1

HCID 68333Dibutyl carbonate

Reagents, catalysts & solvents 1

HCID 2631-ButanolSolvent

Conditions

Temperature
5 °C

Procedure

The operation was performed for 80 hours in the same apparatuses and procedure as in Example 1 except that butyl allophanate was cooled to 5° C. to deposit in a settling vessel equipped in a lower portion of condenser of distillation column 18 and only butanol was returned to reactor 1 via conduit pipe 22. But, in order to remove butyl allophanate, procedures to withdraw butyl allophanate from the settling vessel every one hour and filter out it from butanol became necessary. The feed rate of urea in a steady state was 73.3 mol/hr, whereas the production rate of dibutyl carbonate to be obtained via reaction liquid withdrawing pipe 14 was 71.1 mol/hr (97.0 mol % to fed urea).

Workup

  1. customwas returned to reactor
  2. customBut, in order to remove butyl allophanate, procedures
  3. customto withdraw butyl allophanate from the settling vessel every one hour
  4. filtrationfilter out it from butanol

Sources & evidence

ORD record
ord-8f18f770af6a4ed885989ede7beb133e
Source dataset
uspto-grants-2002_03
Patent number
US06359163B2

Reaction notes

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