Ammonia → N-(3-Chloropropyl)dibutylamine

HRID 1761259

Reaction equation

HRID 1761259 reaction equation
N.Cl.[CH2:3]([N:7]([CH2:12][CH2:13][CH2:14][CH3:15])[CH2:8][CH2:9][CH2:10][Cl:11])[CH2:4][CH2:5][CH3:6]>>[CH2:3]([N:7]([CH2:12][CH2:13][CH2:14][CH3:15])[CH2:8][CH2:9][CH2:10][Cl:11])[CH2:4][CH2:5][CH3:6]

Participants

3

Reactant 2

HCID 222AmmoniaHCID 225950531-Dibutylamino-3-chloropropane hydrochloride

Product 1

HCID 96084N-(3-Chloropropyl)dibutylamine

Procedure

288.4 g (3.392 mol) of 20% aqueous ammonia are introduced into a 1 l reactor and then 618 g (1.696 mol) of 1-dibutylamino-3-chloropropane hydrochloride (assay 66.5%) are added over 10 minutes and at ambient temperature (22±2° C.). The mixture is stirred for 45 minutes at ambient temperature and is left to separate by settling for 30 minutes. The lower aqueous phase (pH=11) is removed and the organic phase is washed with 300 ml of deionized water at ambient temperature. Stirring is carried out for 30 minutes, separation by settling is carried out for 30 minutes and the lower aqueous phase (pH=9) is removed.

Workup

  1. waitis left
  2. customto separate
  3. waitby settling for 30 minutes
  4. customThe lower aqueous phase (pH=11) is removed
  5. washthe organic phase is washed with 300 ml of deionized water at ambient temperature
  6. stirringStirring
  7. waitis carried out for 30 minutes
  8. customseparation
  9. waitby settling is carried out for 30 minutes
  10. customthe lower aqueous phase (pH=9) is removed

Sources & evidence

ORD record
ord-bb17d9151b89419ead2e5b65b31d58b1
Source dataset
uspto-grants-2005_01
Patent number
US06846936B2

Linked notes

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