Water → HCID 13235939, compound

HRID 2164496Notes

Reaction equation

HRID 2164496 reaction equation
[NH2:1][C:2]1[CH:6]=[C:5]([C:7]([CH3:10])([CH3:9])[CH3:8])[NH:4][N:3]=1.[C:11](OC(=O)C)(=[O:13])[CH3:12].O>C1C=CC=CC=1>[C:11]([NH:1][C:2]1[CH:6]=[C:5]([C:7]([CH3:10])([CH3:9])[CH3:8])[NH:4][N:3]=1)(=[O:13])[CH3:12]

Participants

5

Reactant 3

HCID 962Water2×HCID 7918Acetic AnhydrideHCID 5227873-Amino-5-tert-butylpyrazole

Product 1

HCID 13235939HCID 13235939, compoundYield 62.6%

Reagents, catalysts & solvents 1

HCID 241BenzeneSolvent

Procedure

42 g (0.3 mole) of 3-amino-5-t-butylpyrazole prepared in Example 1 was dissolved in 200 ml of benzene, and 30.6 g of acetic anhydride was added dropwise thereto at 20° to 40° C. while cooling with water. After completion of the dropwise addition, the mixture was allowed to react at 50° to 60° C. for 3 hours. Thereafter, the reaction product was cooled, and water was added to form a precipitate. The precipitate was collected by filtration, and washed with water and benzene to obtain 34 g of 3-acetylamino-5-t-butylpyrazole. This product was recrystallized from hydrous methanol and found to have a melting point of 194° to 195° C.

Workup

  1. additionAfter completion of the dropwise addition
  2. customto react at 50° to 60° C. for 3 hours
  3. temperatureThereafter, the reaction product was cooled
  4. customto form a precipitate
  5. filtrationThe precipitate was collected by filtration
  6. washwashed with water and benzene

Sources & evidence

ORD record
ord-7eec0216a14243e7b95ae30c8df51148
Source dataset
uspto-grants-1985_03
Patent number
US04505739

Reaction notes

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