Sulfuric Acid → HCID 54093360, compound

HRID 1742071Notes

Reaction equation

HRID 1742071 reaction equation
[NH2:1][C:2]1[N:6]([C:7](=[N:21][O:22][S:23]([C:26]2[CH:32]=[CH:31][C:29]([CH3:30])=[CH:28][CH:27]=2)(=[O:25])=[O:24])[CH2:8][CH2:9][N:10]2[C:14](=[O:15])[C:13]3=[CH:16][CH:17]=[CH:18][CH:19]=[C:12]3[C:11]2=[O:20])[N:5]=[C:4]([CH3:33])[C:3]=1[Cl:34].S(=O)(=O)(O)O>CC(OC(C)=O)=O.CO>[C:14]([N:1]([C:11](=[O:20])[CH3:12])[C:2]1[N:6]([C:7](=[N:21][O:22][S:23]([C:26]2[CH:27]=[CH:28][C:29]([CH3:30])=[CH:31][CH:32]=2)(=[O:24])=[O:25])[CH2:8][CH2:9][N:10]2[C:11](=[O:20])[C:12]3=[CH:19][CH:18]=[CH:17][CH:16]=[C:13]3[C:14]2=[O:15])[N:5]=[C:4]([CH3:33])[C:3]=1[Cl:34])(=[O:15])[CH3:13]

Participants

5

Reactant 2

HCID 1118Sulfuric AcidHCID 54320777HCID 54320777, compound

Product 1

HCID 54093360HCID 54093360, compoundYield 94.5%

Reagents, catalysts & solvents 2

HCID 887MethanolSolvent2×HCID 7918Acetic AnhydrideSolvent

Procedure

2.62 g (5.2 mmol) of 5-amino-4-chloro-3-methyl-1-(3-phthalimido-O-tosyl-propanehydroximoyl)pyrazole in 15 ml of acetanhydride, to which 0.15 ml of concentrated sulphuric acid has been added, are heated to boiling point and then cooled down. After careful hydrolysis the solid obtained is ground up with methanol and boiled in methanol. The crystals which are produced are filtered off under suction and washed with a little methanol. 1.44 g (47%) of 5-bisacetylamino-4-chloro-3-methyl-1-(3-phthalimido-O-tosyl-propanehydroximoyl)pyrazole with a m. pt. of 143°-147° C. are obtained.

Workup

  1. temperatureare heated
  2. temperaturecooled down
  3. customAfter careful hydrolysis the solid
  4. customobtained
  5. customThe crystals which are produced
  6. filtrationare filtered off under suction
  7. washwashed with a little methanol

Sources & evidence

ORD record
ord-8d5d84cad0644fa0b3574ca2f072894a
Source dataset
uspto-grants-1994_08
Patent number
US05336780

Reaction notes

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