Ammonia → N-(3-Chloropropyl)dibutylamine

HRID 2306864

Reaction equation

HRID 2306864 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

Into a 1 l reactor, there are introduced 288.4 g (3.392 mol) of 20% aqueous ammonia, and then there are added, over 10 minutes and at room temperature (22±2° C.), 618 g (1.696 mol) of 1-dibutylamino-3-chloropropane hydrochloride (titer 66.5%). The medium is stirred for 45 minutes at room temperature and it is allowed to separate by settling for 30 minutes. The bottom aqueous phase (pH=11) is removed, and the organic phase is washed with 300 ml of deionized water at room temperature. The medium is stirred for 30 minutes, separated by settling for 30 minutes and the bottom aqueous phase (pH=9) is drawn off.

Workup

  1. customto separate
  2. waitby settling for 30 minutes
  3. customThe bottom aqueous phase (pH=11) is removed
  4. washthe organic phase is washed with 300 ml of deionized water at room temperature
  5. stirringThe medium is stirred for 30 minutes
  6. customseparated
  7. waitby settling for 30 minutes

Sources & evidence

ORD record
ord-72bf16cc4c354e359ab896c309117a91
Source dataset
uspto-grants-2004_12
Patent number
US06828448B2

Linked notes

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