Sodium Hydroxide → HCID 13588903, compound

HRID 1589168Notes

Reaction equation

HRID 1589168 reaction equation
[Br:1][C:2]1[CH:10]=[CH:9][C:5]([C:6](Cl)=[O:7])=[CH:4][CH:3]=1.Cl.Cl.[N:13]1([CH2:18][CH2:19][NH2:20])[CH:17]=[N:16][CH:15]=[N:14]1.[OH-].[Na+]>C(Cl)Cl>[Br:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([NH:20][CH2:19][CH2:18][N:13]2[CH:17]=[N:16][CH:15]=[N:14]2)=[O:7])=[CH:4][CH:3]=1

Participants

5

Reactant 3

HCID 14798Sodium Hydroxide2×HCID 685154-Bromobenzoyl chlorideHCID 202483172-(1H-1,2,4-triazol-1-yl)ethan-1-amine dihydrochloride

Product 1

HCID 13588903HCID 13588903, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent2×

Procedure

A mixture of about 2.2 g of 4-bromobenzoyl chloride, about 1.85 g of 1H-1,2,4-triazole-1-ethanamine dihydrochloride, about 30 ml of approximately 1N sodium hydroxide and about 75 ml of methylene chloride was stirred overnight, then about 5 ml of approximately 1N sodium hydroxide and about 75 ml of methylene chloride were added. The layers were separated and the organic layer was concentrated to remove the solvent. The crystalline residue was washed onto a filter with ether giving the desired product, mp 160°-162° C.

Workup

  1. customThe layers were separated
  2. concentrationthe organic layer was concentrated
  3. customto remove the solvent
  4. washThe crystalline residue was washed onto
  5. filtrationa filter with ether giving the desired product, mp 160°-162° C.

Sources & evidence

ORD record
ord-86262e30502a4fde9c5178cfcb9d3f25
Source dataset
uspto-grants-1986_02
Patent number
US04568685

Reaction notes

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