Water → HCID 86733843, compound

HRID 1283548Notes

Reaction equation

HRID 1283548 reaction equation
[CH2:1]([CH2:8][NH:9][C:10]([CH3:14])([CH3:13])[C:11]#[N:12])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O>CCOCC>[CH2:1]([CH2:8][NH:9][C:10]([CH3:14])([CH3:13])[CH2:11][NH2:12])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Participants

4

Reactant 2

HCID 962WaterHCID 214098442-Benzylmethylamino-2-methylpropionitrile

Product 1

HCID 86733843HCID 86733843, compoundYield 55.5%

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent2×

Procedure

A solution of 2-benzylmethylamino-2-methyl-propionitrile (6.7 g.) in ether (100 ml.) was added dropwise to a stirred solution of sodium dihydro bis[2-methoxyethoxy] aluminate (28.5 g.) in ether (150 ml.), kept at 0°C. The mixture was then gently refluxed for 20 hrs, and then excess reducing agent was decomposed by the dropwise addition of water to the cooled suspension. The mixture was dried (anhyd.Na2SO4), filtered (hyflo) and the excess ether evaporated under reduced pressure. The residual liquid was distilled under water pump vacuum to give 2-benzylmethylamino-2-methyl-propylamine (3.8 g.) b.p. 138°-140°C.

Workup

  1. customkept at 0°C
  2. temperatureThe mixture was then gently refluxed for 20 hrs
  3. dry with materialThe mixture was dried (anhyd.Na2SO4)
  4. filtrationfiltered (hyflo)
  5. customthe excess ether evaporated under reduced pressure
  6. distillationThe residual liquid was distilled under water

Sources & evidence

ORD record
ord-ff6a65489c1141048ea81a6f41cbcb81
Source dataset
uspto-grants-1976_08
Patent number
US03975443

Reaction notes

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