Methyl triflate → HCID 14324123, compound

HRID 543082Notes

Reaction equation

HRID 543082 reaction equation
[CH3:1][O:2][C:3]1[C:4]([O:13][CH3:14])=[CH:5][C:6]2[Te:10][C:9]([CH3:11])=[N:8][C:7]=2[CH:12]=1.[F:15][C:16]([F:23])([F:22])[S:17]([O:20]C)(=[O:19])=[O:18]>ClCCl>[F:15][C:16]([F:23])([F:22])[S:17]([O-:20])(=[O:19])=[O:18].[CH3:1][O:2][C:3]1[C:4]([O:13][CH3:14])=[CH:5][C:6]2[Te:10][C:9]([CH3:11])=[N+:8]([CH3:16])[C:7]=2[CH:12]=1

Participants

4

Reactant 2

HCID 9526Methyl triflateHCID 139312085,6-Dimethoxy-2-methylbenzotellurazole

Product 1

HCID 14324123HCID 14324123, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

5,6-Dimethoxy-2-methylbenzotellurazole (Example 19) (4.8 g=0.013 mole) was dissolved in dichloromethane (75 ml), and methyl trifluoromethanesulfonate (2.48 g=1.66 ml=0.013 mole) was added. The solution turned cloudy and crystals started to deposit within a few minutes. Precipitation was completed by addition of diethyl ether. The product was collected by filtration to give 5.5 g, 86.5% of theory, m.p. 210°-234° C. The product was recrystallized from boiling acetone (≃130 ml required) m.p. 242°-243° C.

Workup

  1. waitto deposit within a few minutes
  2. customPrecipitation
  3. additionwas completed by addition of diethyl ether
  4. filtrationThe product was collected by filtration
  5. customto give 5.5 g, 86.5% of theory, m.p. 210°-234° C
  6. customThe product was recrystallized

Sources & evidence

ORD record
ord-f8ebe190b7ac42c2b8dd879ace9beea9
Source dataset
uspto-grants-1987_04
Patent number
US04661438

Reaction notes

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