Hydrochloric Acid → HCID 23325982, compound

HRID 2164662Notes

Reaction equation

HRID 2164662 reaction equation
[CH3:1][N:2]([CH2:4][CH2:5][NH:6][C:7]([NH:9][CH2:10][CH2:11][N:12]([CH3:14])[CH3:13])=[O:8])[CH3:3].[ClH:15]>O>[ClH:15].[ClH:15].[CH3:13][N:12]([CH3:14])[CH2:11][CH2:10][NH:9][C:7]([NH:6][CH2:5][CH2:4][N:2]([CH3:3])[CH3:1])=[O:8]

Participants

4

Procedure

A one-liter, four-necked reaction flask fitted with a reflux condenser, mechanical stirrer, thermometer and a dropping funnel was charged with 101.1 g (0.5 mole) of 1,3-bis(2-dimethylaminoethyl)urea prepared in Example 1 and 167.7 g of water. The solution was chilled by immersion in an ice-water bath, and 98.7 g (1.0 mole) 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(2-dimethylaminoethyl)urea dihydrochloride solution so obtained, 92.5 g (1.0 mole) 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 30 minutes and then heated at 70° C. for another 30 minutes. A 50 percent aqueous solution of the title compound was obtained.

Workup

  1. customA one-liter, four-necked reaction flask fitted with a reflux condenser, mechanical stirrer
  2. temperatureThe solution was chilled by immersion in an ice-water bath
  3. customthe temperature below 48° C

Sources & evidence

ORD record
ord-b3eb42a1aaf540349b09c825acc1d34b
Source dataset
uspto-grants-1985_03
Patent number
US04506081

Reaction notes

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