Hydrochloric Acid → HCID 20199958, compound

HRID 1380214Notes

Reaction equation

HRID 1380214 reaction equation
[CH3:1][N:2]([CH2:4][CH2:5][CH2:6][NH:7][C:8]([NH:10][CH2:11][CH2:12][CH2:13][N:14]([CH3:16])[CH3:15])=[O:9])[CH3:3].[ClH:17]>>[ClH:17].[ClH:17].[CH3:16][N:14]([CH2:13][CH2:12][CH2:11][NH:10][C:8]([NH:7][CH2:6][CH2:5][CH2:4][N:2]([CH3:1])[CH3:3])=[O:9])[CH3:15]

Participants

3

Reactant 2

HCID 313Hydrochloric AcidHCID 1041631,3-Bis(3-(dimethylamino)propyl)urea

Product 1

HCID 20199958HCID 20199958, compound

Procedure

A five-liter, four-necked reaction flask fitted with a reflux condenser, mechanical stirrer, thermometer and a dropping funnel was charged with 996.6 g (4.0 moles) of 1,3-bis(dimethylaminopropyl)urea of 92.5 percent purity. This compound was prepared by the method described in U.S. Pat. No. 4,157,388. The contents of the flask were chilled by immersion into an ice-water bath, and 788.4 g (8.0 moles) of 37 percent hydrochloric acid was added at such a rate as to keep the temperature below 48° C. To the well-agitated 1,3-bis(dimethylaminopropyl)urea dihydrochloride solution so obtained, 740.0 g (8.0 moles) of epichlorohydrin was added slowly, taking care that the temperature did not exceed 48° C. After this addition was completed, the solution was kept at 45°-48° C. for one-half hour and then heated at 70° C. for another 30 minutes. A 77.3 percent equeous solution of the title compound was obtained.

Workup

  1. customA five-liter, four-necked reaction flask fitted with a reflux condenser, mechanical stirrer
  2. customThis compound was prepared by the method
  3. temperatureThe contents of the flask were chilled by immersion into an ice-water bath
  4. customthe temperature below 48° C

Sources & evidence

ORD record
ord-4cac9c54ab954965b1c66832b95427c3
Source dataset
uspto-grants-1986_04
Patent number
US04581058

Reaction notes

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