Acetic Anhydride → HCID 15580722, compound

HRID 543811Notes

Reaction equation

HRID 543811 reaction equation
F[C:2](F)(F)[C:3]([NH:5][C:6]1[CH2:10][CH:9]([CH3:11])[N:8]([C:12]2[CH:17]=[CH:16][C:15](C(=O)C(F)(F)F)=[CH:14][CH:13]=2)[N:7]=1)=[O:4].C(OC(=O)C)(=O)C>CN(C)C1C=CN=CC=1.ClCCl>[CH3:11][CH:9]1[N:8]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[N:7]=[C:6]([NH:5][C:3](=[O:4])[CH3:2])[CH2:10]1

Participants

5

Reactant 2

HCID 7918Acetic AnhydrideHCID 15580702HCID 15580702, compound

Product 1

HCID 15580722HCID 15580722, compound

Reagents, catalysts & solvents 2

HCID 142844-(Dimethylamino)pyridineCatalystHCID 6344DichloromethaneSolvent

Procedure

A mixture of 2.0 g. of 3-amino-5-methyl-1-phenyl-2-pyrazoline (prepared in Example 5), 5.0 ml. of acetic anhydride and 100 mg. of 4-dimethylaminopyridine is allowed to stand at room temperature for 3 hours. The mixture is filtered to give a white solid. The solid is dissolved in dichloromethane and is columnized and recrystallized as for Example 14 (B) to give 0.90 g. of the desired product as colorless plates, m.p. 144.5°-146.5° C.

Workup

  1. additionA mixture of 2.0 g
  2. filtrationThe mixture is filtered
  3. customto give a white solid
  4. customto give 0.90 g

Sources & evidence

ORD record
ord-126f2227b75e4ea69b32c29420fcfdcf
Source dataset
uspto-grants-1984_05
Patent number
US04447442

Reaction notes

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