Hydrochloric Acid → HCID 19845271, compound

HRID 543072Notes

Reaction equation

HRID 543072 reaction equation
[Cl:1][TeH:2]1(Cl)(Cl)[C:7]2[CH:8]=[CH:9][C:10]([OH:12])=[CH:11][C:6]=2[NH+:5]=[C:4]([CH3:13])O1.[OH-].[Na+].[BH4-].[Na+].Cl>CO.O>[Cl-:1].[OH:12][C:10]1[CH:9]=[CH:8][C:7]2[Te:2][CH:4]([CH3:13])[NH2+:5][C:6]=2[CH:11]=1

Participants

7

Reactant 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 4311764Sodium borohydrideHCID 131715117HCID 131715117, compound

Product 1

HCID 19845271HCID 19845271, compound

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 962WaterSolvent

Procedure

1,1,1-Trichloro-6-hydroxy-3-methyl-2,1,4-benzoxatellurazinium, inner salt (Example 11) (19.2 g=0.05 mole) was dissolved in methanol (200 ml) with addition of sodium hydroxide (4 g) in water (20 ml). The reduction was carried out under a nitrogen atmosphere, using sodium borohydride (4.3 g=0.11 mole), after the addition of which the solution became clear. The reaction mixture was cooled to ≃10° C., and concentrated hydrochloric acid (65 ml) was added in one portion. Considerable black precipitate (11.7 g) formed, which was collected by filtration. The filtrate was evaporated to 50 ml and chilled to give a second crop (12.3 g). The products were recrystallized from isopropanol to give a combined yield of 9.45 g, 63.9% of theory, cream colored powder, m.p. 125°-132° C. (dec.).

Workup

  1. additionafter the addition of which the solution
  2. temperatureThe reaction mixture was cooled
  3. customto ≃10° C.

Sources & evidence

ORD record
ord-2d6d714b5ed7415c869f1363ea5ef63d
Source dataset
uspto-grants-1987_04
Patent number
US04661438

Reaction notes

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