2-Butanamine, 2-methyl- → HCID 43199060, compound

HRID 539429Notes

Reaction equation

HRID 539429 reaction equation
Cl.[Cl-].[CH3:3][N:4]([CH3:7])[CH2:5][CH3:6].[C:8]([NH2:13])([CH2:11][CH3:12])([CH3:10])[CH3:9]>>[C:8]([NH:13][CH2:6][CH2:5][N:4]([CH3:7])[CH3:3])([CH2:11][CH3:12])([CH3:10])[CH3:9]

Participants

3

Procedure

Into a 300 mL-volume flask equipped with a stirrer and a thermometer were placed 20.6 g (143 mmol) of 2-(dimethylamino)ethane chloride hydrochloride and 74.0 g (859 mmol) of t-pentylamine. And then, the mixture was heated to reflux for 8 hours. After the completion of the reaction, the reaction mixture was filtrated and washed with 100 ml of hexane twice, and the hexane layer was concentrated under reduced pressure. The resultant concentrate was distilled under reduced pressure (120° C., 11.0 kPa), to provide 13.5 g of 1-t-pentylamino-2-dimethylaminoethane. (Isolation yield: 60%)

Workup

  1. customInto a 300 mL-volume flask equipped with a stirrer
  2. temperatureAnd then, the mixture was heated
  3. temperatureto reflux for 8 hours
  4. customAfter the completion of the reaction
  5. filtrationthe reaction mixture was filtrated
  6. washwashed with 100 ml of hexane twice
  7. concentrationthe hexane layer was concentrated under reduced pressure
  8. concentrationThe resultant concentrate
  9. distillationwas distilled under reduced pressure (120° C., 11.0 kPa)

Sources & evidence

ORD record
ord-18f2d0f377bf41a2b7c956520200885d
Source dataset
uspto-grants-2014_10
Patent number
US08871304B2

Reaction notes

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