HCID 15580707, compound → HCID 15580720, compound

HRID 543804Notes

Reaction equation

HRID 543804 reaction equation
[Cl:1][C:2]1[CH:3]=[C:4]([N:9]2[CH2:13][CH2:12][C:11]([NH:14][C:15](=[O:20])C(F)(F)F)=[N:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8].ClC1C=C(N2CC(C)C(NC=O)=N2)C=CC=1Cl>C(O)=O>[Cl:1][C:2]1[CH:3]=[C:4]([N:9]2[CH2:13][CH2:12][C:11]([NH:14][CH:15]=[O:20])=[N:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8]

Participants

4

Reactant 2

HCID 15580707HCID 15580707, compoundHCID 15580721HCID 15580721, compound

Product 1

HCID 15580720HCID 15580720, compound

Reagents, catalysts & solvents 1

HCID 284Formic AcidSolvent

Procedure

A mixture of 5.0 g. of 3-amino-1-(3,4-dichlorophenyl)-2-pyrazoline (prepared in Example 1) and 25 ml. of a mixture of formic acid and acetic anhydride (Example 15) is allowed to stand at room temperature for one hour. The resulting solid is collected by filtration and washed with hexane. The solid is dissolved in dichloromethane and is columnized and recrystallized as described in Example 5 to give 3.85 g. of the desired product as yellow prisms, m.p. 151°-153° C.

Workup

  1. additionA mixture of 5.0 g
  2. filtrationThe resulting solid is collected by filtration
  3. washwashed with hexane
  4. dissolutionThe solid is dissolved in dichloromethane
  5. customrecrystallized
  6. customto give 3.85 g

Sources & evidence

ORD record
ord-a3936648f46947568829f3767ab788d1
Source dataset
uspto-grants-1984_05
Patent number
US04447442

Reaction notes

Loading…