Sodium Bicarbonate → HCID 13931216, compound

HRID 543076Notes

Reaction equation

HRID 543076 reaction equation
[Cl-].[CH3:2][CH:3]1[NH2+:7][C:6]2[CH:8]=[C:9]([S:12][CH3:13])[CH:10]=[CH:11][C:5]=2[Te:4]1.C(=O)(O)[O-].[Na+]>O>[CH3:2][C:3]1[Te:4][C:5]2[CH:11]=[CH:10][C:9]([S:12][CH3:13])=[CH:8][C:6]=2[N:7]=1

Participants

4

Reactant 2

HCID 516892Sodium BicarbonateHCID 86741446HCID 86741446, compound

Product 1

HCID 13931216HCID 13931216, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

2-Methyl-5-methylthiobenzotellurazolium chloride (Example 16) (11.5 g=0.035 mole) was suspended in water and sodium bicarbonate in excess of that stoichiometrically required was added. The free base was extracted into dichloromethane. The organic solution was washed with saturated aqueous sodium sulfate, dried, and evaporated in vacuum to a yellow oil (9.06 g). Upon addition of isopropanol (40 ml) the oil crystallized spontaneously to almost white needles to give 8.18 g, 79.8% of theory, m.p. 64°-67° C.

Workup

  1. extractionThe free base was extracted into dichloromethane
  2. washThe organic solution was washed with saturated aqueous sodium sulfate
  3. customdried
  4. customevaporated in vacuum to a yellow oil (9.06 g)
  5. additionUpon addition of isopropanol (40 ml) the oil
  6. customcrystallized spontaneously to almost white needles
  7. customto give 8.18 g, 79.8% of theory, m.p. 64°-67° C.

Sources & evidence

ORD record
ord-bb7f1b8f8c9345ca9830f6e2f31f2ea4
Source dataset
uspto-grants-1987_04
Patent number
US04661438

Reaction notes

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