Ammonia → HCID 70045731, compound

HRID 2351948Notes

Reaction equation

HRID 2351948 reaction equation
[CH:1]1([NH:6][C:7](=[O:12])[CH2:8][C:9]([CH3:11])=O)[CH2:5][CH2:4][CH2:3][CH2:2]1.[NH3:13]>C(O)C>[CH:1]1([NH:6][C:7](=[O:12])/[CH:8]=[C:9](\[NH2:13])/[CH3:11])[CH2:5][CH2:4][CH2:3][CH2:2]1

Participants

4

Reactant 2

HCID 222Ammonia2×HCID 25248858102-45-7

Product 1

HCID 70045731HCID 70045731, compoundYield 85.6%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

Acetoacetic cyclopentylamide (169.1 g, 1.00 mole) is dissolved in ethanol (100 ml) and thereto is passed ammonia gas, while the temperature is controlled below 30° C. by cooling with a water bath. After passing ammonia gas for about 3 hours, colorless crystals precipitate. The reaction mixture is allowed to stand at 0° C. overnight. The precipitates are separated by filtration and washed with diethyl ether to give the title compound (140.4 g, yield 85.6%) as colorless needles, m.p. 138°-139° C.

Workup

  1. customis controlled below 30° C.
  2. temperatureby cooling with a water bath
  3. customfor about 3 hours
  4. customThe precipitates are separated by filtration
  5. washwashed with diethyl ether

Sources & evidence

ORD record
ord-c8b1073d19ea42159a05e106ba978c6a
Source dataset
uspto-grants-1989_10
Patent number
US04874773

Reaction notes

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