Formaldehyde → HCID 15718283, compound

HRID 2107962Notes

Reaction equation

HRID 2107962 reaction equation
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[CH2:14]=[O:15]>C(O)(=O)C>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([CH2:2][C:1]([CH3:4])([CH3:3])[CH2:14][OH:15])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]

Participants

4

Reactant 2

HCID 712FormaldehydeHCID 143452tert-Butyl piperazine-1-carboxylate

Product 1

HCID 15718283HCID 15718283, compoundYield 94%

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Procedure

2.9 g of N-(tert-butyloxycarbonyl)piperazine and 1.6 ml of 35% formalin were dissolved in 8 ml of acetic acid, and the resulting solution was stirred at room temperature for 30 minutes. Then, 1.5 ml of isobutylaldehyde was added, and the resulting mixture was stirred at 50° C. for 12 hours. After concentration under reduced pressure, the residue was extracted with ethyl acetate and washed with saturated aqueous sodium bicarbonate. After drying with anhydrous sodium sulfate, the solvent was evaporated under reduced pressure to give 3.9 g of a colorless powdery crystal (yield: 94%). The IR and NMR data of the compound thus obtained are as follows: ##STR51##

Workup

  1. stirringthe resulting mixture was stirred at 50° C. for 12 hours
  2. concentrationAfter concentration under reduced pressure
  3. extractionthe residue was extracted with ethyl acetate
  4. washwashed with saturated aqueous sodium bicarbonate
  5. dry with materialAfter drying with anhydrous sodium sulfate
  6. customthe solvent was evaporated under reduced pressure

Sources & evidence

ORD record
ord-f37730ef3b7247d7967e9b8641522a3c
Source dataset
uspto-grants-1990_06
Patent number
US04937242

Reaction notes

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