Tert-Butylamine → 1,2-Ethanediamine,N2-(1,1-dimethylethyl)-N1,N1-dimethyl-

HRID 539428Notes

Reaction equation

HRID 539428 reaction equation
[C:1]([NH2:5])([CH3:4])([CH3:3])[CH3:2].Cl.[CH3:7][N:8]([CH3:12])[CH2:9][CH2:10]Cl>O>[C:1]([NH:5][CH2:10][CH2:9][N:8]([CH3:12])[CH3:7])([CH3:4])([CH3:3])[CH3:2]

Participants

4

Procedure

Into a 50 mL-volume flask equipped with a stirrer, a thermometer and a dropping funnel were placed 16 g (0.22 mol) of t-butylamine, 5.0 g (35 mmol) of 2-(dimethylamino)ethyl chloride hydrochloride and 1 ml of water. And then, the mixture was reacted at 70° C. for 10 hours. After the completion of the reaction, the reaction solution was subjected to extraction with 25 ml of hexane twice, and the hexane layer was concentrated under reduced pressure. The resultant concentrate was distilled under reduced pressure (60° C., 2.4 kPa), to provide 3.0 g of 1-(t-butylamino)-2-dimethylaminoethane. (Isolation yield: 60%)

Workup

  1. customInto a 50 mL-volume flask equipped with a stirrer
  2. customAnd then, the mixture was reacted at 70° C. for 10 hours
  3. customAfter the completion of the reaction
  4. extractionthe reaction solution was subjected to extraction with 25 ml of hexane twice
  5. concentrationthe hexane layer was concentrated under reduced pressure
  6. concentrationThe resultant concentrate
  7. distillationwas distilled under reduced pressure (60° C., 2.4 kPa)

Sources & evidence

ORD record
ord-0f1ace3313dd47cc9ac6e6adfacd7ea5
Source dataset
uspto-grants-2014_10
Patent number
US08871304B2

Reaction notes

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