Water → HCID 300609, compound

HRID 1740847Notes

Reaction equation

HRID 1740847 reaction equation
[CH2:1]([NH:4][CH2:5][CH2:6][CH3:7])[CH2:2][CH3:3].C(N([CH2:13][CH3:14])CC)C.C(Cl)Cl.CC[C:20]([C:22](Cl)=[O:23])=[O:21].[OH2:25]>>[O:21]=[C:20]([N:4]([CH2:5][CH2:6][CH3:7])[CH2:1][CH2:2][CH3:3])[C:22]([O:23][CH2:13][CH3:14])=[O:25]

Participants

6

Reactant 5

HCID 962WaterHCID 6344Dichloromethane2×HCID 8471TriethylamineHCID 8902DipropylamineHCID 11007880Butanoyl chloride, 2-oxo-

Product 1

HCID 300609HCID 300609, compound

Procedure

To a mixture of dipropylamine (5.0 g), triethylamine (5.5 g) and methylene chloride (70 ml) is added dropwise a solution of ethyloxalyl chloride (7.4 g) and methylene chloride (30 ml) with stirring while the temperature of the mixture is kept at -20° C. After addition, the mixture is stirred at 0° C. for four hours. To the reaction mixture is added water, and the methylene chloride layer is collected, dried over anhydrous sodium sulfate, and concentrated under reduced pressure to give ethyl 2-oxo-2-(N,N-dipropylamino)acetate (9.5 g) as an oily product.

Workup

  1. customis kept at -20° C
  2. additionAfter addition
  3. stirringthe mixture is stirred at 0° C. for four hours
  4. customthe methylene chloride layer is collected
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated under reduced pressure

Sources & evidence

ORD record
ord-0e53919f7f604c47b35371fa1b041c14
Source dataset
uspto-grants-1999_10
Patent number
US05972946

Reaction notes

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