Dimethylamine → HCID 21917324, compound

HRID 404996Notes

Reaction equation

HRID 404996 reaction equation
[CH3:1][NH:2][CH3:3].[C:4]([OH:9])(=[O:8])/[CH:5]=[CH:6]/[CH3:7]>>[CH3:1][NH:2][CH3:3].[C:4]([OH:9])(=[O:8])/[CH:5]=[CH:6]/[CH3:7]

Participants

3

Reactant 2

HCID 674DimethylamineHCID 637090Crotonic Acid3×

Product 1

HCID 21917324HCID 21917324, compound

Procedure

Dimethylamine (30 g) was added to a pressure-resistant container (reactor), and the reactor was hermetically sealed. The temperature of the reactor was adjusted to 20° C., and crotonic acid (14.3 g) was fed into the reactor by means of a high-pressure pump. During addition of crotonic acid, heat of neutralization is generated. Therefore, while the reactor was cooled in an ice bath, crotonic acid was added dropwise to the reactor at a rate of 5 to 7 mL/minute, so as to adjust the temperature in the reactor to 25 to 35° C. After completion of dropwise addition, reaction was allowed to proceed for one hour, and then analysis was carried out. The reaction time (as measured from initiation of dropwise addition) was one hour and three minutes.

Workup

  1. customthe reactor was hermetically sealed
  2. customwas adjusted to 20° C.
  3. temperatureheat of neutralization
  4. temperatureTherefore, while the reactor was cooled in an ice bath
  5. customto 25 to 35° C
  6. additionAfter completion of dropwise addition, reaction
  7. additionThe reaction time (as measured from initiation of dropwise addition)
  8. waitwas one hour and three minutes

Sources & evidence

ORD record
ord-5fa4fc3690fb4615916290eead40de16
Source dataset
uspto-grants-2014_06
Patent number
US08748659B2

Reaction notes

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