Dichloromethane → HCID 178526434, compound

HRID 1586360Notes

Reaction equation

HRID 1586360 reaction equation
[N+:1]([O-:4])([O-])=[O:2].[K+].[F:6][C:7]1([F:21])[O:11][C:10]2[CH:12]=[CH:13][CH:14]=[C:15]([C:16]3[CH:20]=[CH:19][NH:18][N:17]=3)[C:9]=2[O:8]1.C(Cl)[Cl:23]>OS(O)(=O)=O>[Cl:23][C:20]1[C:16]([C:15]2[C:9]3[O:8][C:7]([F:6])([F:21])[O:11][C:10]=3[CH:12]=[CH:13][C:14]=2[N+:1]([O-:4])=[O:2])=[N:17][NH:18][CH:19]=1

Participants

5

Reactant 3

HCID 6344DichloromethaneHCID 24434Potassium NitrateHCID 178506006HCID 178506006, compound

Product 1

HCID 178526434HCID 178526434, compoundYield 63%

Reagents, catalysts & solvents 1

HCID 1118Sulfuric AcidSolvent

Conditions

Temperature
0 °C

Procedure

6.3 g (0.063 mol) of KNO3 are added, in small portions and at 0° C., to 12.8 g of 1-(acetyl),4-chloro, 3-(2,2-difluorobenzo-1,3-dioxol-4-yl)pyrazole dissolved in 21 ml of H2SO4 (96%) and 140 ml of CH2Cl2. The reaction mixture is stirred for 3 h at 0° C. and then poured poured onto 300 cm3 of ice. The precipitate is recovered by filtration, washed with water and then heptane and dried. We obtain 8.05 g of 4-chloro-3-(2,2-difluoro-5-nitrobenzo-1,3-dioxol-4-yl)pyrazole melting at 180° C. (yield 63%).

Workup

  1. additionpoured
  2. filtrationThe precipitate is recovered by filtration
  3. washwashed with water
  4. dry with materialheptane and dried

Sources & evidence

ORD record
ord-713ea1d21a174042a72df8533821c09b
Source dataset
uspto-grants-1999_08
Patent number
US05945382

Reaction notes

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