HCID 12317882, compound → HCID 12317883, compound

HRID 437772Notes

Reaction equation

HRID 437772 reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:14]2[CH:15]=[C:16]([NH:19][OH:20])[CH:17]=[CH:18][C:13]=2[N:12]2[C:21]([CH3:24])=[N:22][N:23]=[C:11]2[CH2:10][N:9]=1>C(Cl)Cl.[O-2].[O-2].[Mn+4]>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:14]2[CH:15]=[C:16]([N:19]=[O:20])[CH:17]=[CH:18][C:13]=2[N:12]2[C:21]([CH3:24])=[N:22][N:23]=[C:11]2[CH2:10][N:9]=1

Participants

4

Reactant 1

HCID 12317882HCID 12317882, compound

Product 1

HCID 12317883HCID 12317883, compound

Reagents, catalysts & solvents 2

HCID 178418406HCID 178418406, compoundCatalyst2×HCID 6344DichloromethaneSolvent

Procedure

Manganese dioxide, 20 g, was added to a suspension of 2 g of 6-(2-chlorophenyl)-8-hydroxyamino-1-methyl-4H-s-triazolo-[4,3-a][1,4]benzodiazepine in 1 l of methylene chloride. After stirring for 3 hr at room temperature the manganese dioxide was separated by filtration over celite. The filtrate was evaporated and the residue was crystallized from methylene chloride/ether to yield the above-named product, with mp. 190°-195° dec. For analysis it was recrystallized from ethanol/ether.

Workup

  1. customwas separated by filtration over celite
  2. customThe filtrate was evaporated
  3. customthe residue was crystallized from methylene chloride/ether
  4. customto yield the above-named product
  5. customFor analysis it was recrystallized from ethanol/ether

Sources & evidence

ORD record
ord-c0819a47e18245fd80a9fc8da63ecef9
Source dataset
uspto-grants-1977_06
Patent number
US04032535

Reaction notes

Loading…