Hydrochloric Acid → HCID 19845293, compound

HRID 543070Notes

Reaction equation

HRID 543070 reaction equation
[Cl:1][TeH:2]1(Cl)(Cl)[C:7]2[CH:8]=[CH:9][C:10]([CH3:12])=[CH:11][C:6]=2[NH+:5]=[C:4]([CH3:13])O1.[OH-].[Na+].[BH4-].[Na+].Cl>CO>[Cl-:1].[CH3:13][CH:4]1[NH2+:5][C:6]2[CH:11]=[C:10]([CH3:12])[CH:9]=[CH:8][C:7]=2[Te:2]1

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 4311764Sodium borohydrideHCID 131715113HCID 131715113, compound

Product 1

HCID 19845293HCID 19845293, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

1,1,1-Trichloro-3,6-dimethyl-2,1,4-benzoxatellurazinium, inner salt (Example 8) (17.3 g=0.05 mole) was dissolved in a mixture of methanol (300 ml) and 1N sodium hydroxide (100 ml, 0.1 mole) in a vessel fitted with a nitrogen inlet, a condenser, and a magnetic stirrer. Through the condenser was added sodium borohydride until further addition no longer produced a transient orange color. This required about 3.0 g. The mixture was stirred for a few minutes under nitrogen, then concentrated hydrochloric acid (100 ml) was added in one portion. The mixture was clarified by filtration with Celite®, then evaporated under reduced pressure to 200 ml, again filtered from inorganic salts and chilled overnight. Filtration yielded yield 9.15 g of colorless solid, which was rinsed with isopropanol and air dried. The material was not pure and contained inorganic salt contaminants.

Workup

  1. customfitted with a nitrogen inlet, a condenser, and a magnetic stirrer
  2. additionuntil further addition
  3. customno longer produced a transient orange color
  4. filtrationThe mixture was clarified by filtration with Celite®
  5. customevaporated under reduced pressure to 200 ml
  6. filtrationagain filtered from inorganic salts
  7. temperaturechilled overnight
  8. filtrationFiltration

Sources & evidence

ORD record
ord-34282ae09fdb4ac0bf1eb9640ce249d8
Source dataset
uspto-grants-1987_04
Patent number
US04661438

Reaction notes

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