Sodium Hydroxide → HCID 13588860, compound

HRID 1589165Notes

Reaction equation

HRID 1589165 reaction equation
Cl.Cl.[N:3]1([CH2:8][CH2:9][CH2:10][CH2:11][NH2:12])[CH:7]=[N:6][CH:5]=[N:4]1.[OH-].[Na+].[Cl:15][C:16]1[CH:17]=[C:18]([CH:22]=[CH:23][C:24]=1[Cl:25])[C:19](Cl)=[O:20]>C(Cl)Cl>[Cl:15][C:16]1[CH:17]=[C:18]([CH:22]=[CH:23][C:24]=1[Cl:25])[C:19]([NH:12][CH2:11][CH2:10][CH2:9][CH2:8][N:3]1[CH:7]=[N:6][CH:5]=[N:4]1)=[O:20]

Participants

5

Reactant 3

HCID 14798Sodium Hydroxide2×HCID 76403Benzoyl chloride, 3,4-dichloro-HCID 20266537HCID 20266537, compound

Product 1

HCID 13588860HCID 13588860, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent2×

Procedure

A mixture of about 2.13 g of 1H-1,2,4-triazole-1-butanamine, dihydrochloride, about 75 ml of methylene chloride, about 30 ml of approximately 1N sodium hydroxide and about 1.41 ml of 3,4-dichlorobenzoyl chloride was stirred at room temperature overnight. An additional, about 5 ml of approximately 1N sodium hydroxide and about 50 ml of methylene chloride were added and the layers were separated. The organic layer was washed with water, dried and concentrated. The oil was collected and crystallized from ether, giving about 2.3 g of the desired product as white crystals, mp 97°-99° C.

Workup

  1. customthe layers were separated
  2. washThe organic layer was washed with water
  3. customdried
  4. concentrationconcentrated
  5. customThe oil was collected
  6. customcrystallized from ether

Sources & evidence

ORD record
ord-3b760baf513f48deb7f459535977fac9
Source dataset
uspto-grants-1986_02
Patent number
US04568685

Reaction notes

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