Acetic Anhydride → HCID 53834620, compound

HRID 2120561Notes

Reaction equation

HRID 2120561 reaction equation
C(O[C:5](=[O:7])C)(=O)C.[NH:8]([N:10]=[CH:11][N:12]1[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1)[NH2:9].[OH-].[K+]>C(O)=O>[CH:5]([N:15]1[CH2:16][CH2:17][N:12]([CH:11]=[N:10][NH:8][NH2:9])[CH2:13][CH2:14]1)=[O:7]

Participants

5

Reactant 3

HCID 7918Acetic AnhydrideHCID 14797Potassium HydroxideHCID 54189776HCID 54189776, compound

Product 1

HCID 53834620HCID 53834620, compound

Reagents, catalysts & solvents 1

HCID 284Formic AcidSolvent2×

Procedure

12.7 ml of acetic acid anhydride are added dropwise to 42 ml of ice-cooled formic acid, the mixture is stirred for ca. 1 hour and 16 g of the benzylidene derivative of 1-(hydrazinoimino-methyl) piperazine in 42 ml of formic acid are added dropwise. The mixture is left for ca. 2 hours at 0° and the solvent is evaporated off. The residue is treated with water and the pH of the mixture obtained is adjusted to pH 11 by addition of 10N KOH. The mixture is extracted with dichloromethane, the dichloromethane phase is dried and the solvent is evaporated off. The benzylidene derivative of 1-formyl4-(hydrazinoiminomethyl)piperazine is obtained in the form of a white powder.

Workup

  1. waitThe mixture is left for ca. 2 hours at 0°
  2. customthe solvent is evaporated off
  3. additionThe residue is treated with water
  4. customthe pH of the mixture obtained
  5. extractionThe mixture is extracted with dichloromethane
  6. dry with materialthe dichloromethane phase is dried
  7. customthe solvent is evaporated off

Sources & evidence

ORD record
ord-552774666d2c46b4ac9302341514a90d
Source dataset
uspto-grants-2004_02
Patent number
US06693095B2

Reaction notes

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