Ammonium Hydroxide → 1,2-Diethyl-4-pyrazolidinamine

HRID 1706393Notes

Reaction equation

HRID 1706393 reaction equation
Cl[CH:2]1[CH2:6][N:5]([CH2:7][CH3:8])[N:4]([CH2:9][CH3:10])[CH2:3]1.[OH-].[NH4+:12]>>[NH2:12][CH:2]1[CH2:6][N:5]([CH2:7][CH3:8])[N:4]([CH2:9][CH3:10])[CH2:3]1

Participants

3

Procedure

A mixture of 100 g. (0.615 mole) of 4-chloro-1,2-diethylpyrazolidine and 200 ml. of concentrated ammonium hydroxide in a closed steel chamber was heated at 150° C. for approximately 36 hours. The cooled reaction mixture was extracted with isopropyl ether, the aqueous layer saturated with potassium carbonate and continuously extracted with chloroform for six hours. The dried chloroform extract (sodium sulfate) was concentrated at reduced pressure and the residue distilled at 113°-115° C./40 mm. to give 40.5 g. (45.5%) of product.

Workup

  1. additionA mixture of 100 g
  2. customThe cooled reaction mixture
  3. extractionwas extracted with isopropyl ether
  4. extractionthe aqueous layer saturated with potassium carbonate and continuously extracted with chloroform for six hours
  5. extractionThe dried chloroform extract (sodium sulfate)
  6. concentrationwas concentrated at reduced pressure
  7. distillationthe residue distilled at 113°-115° C./40 mm
  8. customto give 40.5 g

Sources & evidence

ORD record
ord-8f2a4e9863b0401ab2a22d6a422b98fb
Source dataset
uspto-grants-1980_06
Patent number
US04207327

Reaction notes

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