Sodium Hydroxide → HCID 47382, compound

HRID 1439014Notes

Reaction equation

HRID 1439014 reaction equation
[CH:1](=[N:3][C:4]([CH2:11][CH2:12][CH3:13])([CH2:8][CH2:9][CH3:10])[CH2:5][CH2:6][CH3:7])[CH3:2].[BH4-].[Na+].[OH-].[Na+]>CO>[CH2:1]([NH:3][C:4]([CH2:11][CH2:12][CH3:13])([CH2:5][CH2:6][CH3:7])[CH2:8][CH2:9][CH3:10])[CH3:2]

Participants

5

Conditions

Temperature
5 °C

Procedure

Into a 500-ml three-necked flask, fitted with a mechanical stirrer and a condenser, were introduced 17.6 g (0.096 mol) of N-ethylidene-1,1-di-n-propyl-n-butylamine, prepared as described hereabove, and 150 ml of methanol. To this solution when cooled, 7.6 g (0.2 mol) of sodium borohydride were added slowly and while stirring. After this operation, the mixture was maintained at a temperature of 5° C for 30 minutes and then progressively heated under reflux. Thirty minutes later, the methanol was evaporated off under vacuum and 200 ml of water were added to the residue so obtained followed by 100 ml of a solution of sodium hydroxide (d = 1.38). The organic fraction was extracted with ether and the solution was distilled under reduced pressure.

Workup

  1. customInto a 500-ml three-necked flask, fitted with a mechanical stirrer and a condenser
  2. customprepared
  3. temperatureTo this solution when cooled
  4. temperatureprogressively heated
  5. temperatureunder reflux
  6. customThirty minutes later, the methanol was evaporated off under vacuum and 200 ml of water
  7. additionwere added to the residue
  8. customso obtained
  9. extractionThe organic fraction was extracted with ether
  10. distillationthe solution was distilled under reduced pressure

Sources & evidence

ORD record
ord-901b45e328b74e81bbab48f25b057c2b
Source dataset
uspto-grants-1977_11
Patent number
US04057644

Reaction notes

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