Hydrochloric Acid → HCID 15586403, compound

HRID 2290370Notes

Reaction equation

HRID 2290370 reaction equation
[BH4-].[Na+].[CH3:3][C:4]1[C:9]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[N:8][NH:7][C:6](=[S:16])[N:5]=1.Cl>O>[CH3:3][CH:4]1[C:9]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[N:8][NH:7][C:6](=[S:16])[NH:5]1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 4311764Sodium borohydrideHCID 20232127HCID 20232127, compound

Product 1

HCID 15586403HCID 15586403, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

Sodium borohydride (0.71 g) and 5-methyl-6-phenyl-1,2,4-triazine-3(2H)-thione which have methanol of crystallization (4.03 g) were reacted in tetrahydrofuran according to a similar manner to that of EXAMPLE 2:(2). The reaction mixture was treated with a mixture of 1N-hydrochloric acid and water, and then extracted with ethyl acetate. The extract was washed successively with 1N hydrochloric acid, brine, an aqueous solution of sodium carbonate and brine, dried over magnesium sulfate and concentrated to dryness. The resultant solid was washed with diisopropyl ether and recrystallized from ethanol to give 5-methyl-6-phenyl-4,5-dihydro-1,2,4-triazine-3(2H)-thione (1.48 g), mp 213°~214.5° C.

Workup

  1. custommethanol of crystallization (4.03 g)
  2. customwere reacted in tetrahydrofuran according to a similar manner to that of EXAMPLE 2
  3. extractionextracted with ethyl acetate
  4. washThe extract was washed successively with 1N hydrochloric acid, brine
  5. dry with materialan aqueous solution of sodium carbonate and brine, dried over magnesium sulfate
  6. concentrationconcentrated to dryness
  7. washThe resultant solid was washed with diisopropyl ether
  8. customrecrystallized from ethanol

Sources & evidence

ORD record
ord-6f4122bc58574efc8dafdf032de09fb0
Source dataset
uspto-grants-1986_10
Patent number
US04616014

Reaction notes

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