Hydrochloric Acid → HCID 9862025, compound

HRID 10761Notes

Reaction equation

HRID 10761 reaction equation
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]([O:22][Si](C)(C)C)([CH2:16][N:17]1[CH:21]=[N:20][CH:19]=[N:18]1)[CH2:10][N:11]1[CH:15]=[N:14][CH:13]=[N:12]1.CO.Cl>O>[OH2:22].[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]([OH:22])([CH2:16][N:17]1[CH:21]=[N:20][CH:19]=[N:18]1)[CH2:10][N:11]1[CH:15]=[N:14][CH:13]=[N:12]1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 112918882-(2,4-Difluorophenyl)-1,3-bis(1,2,4-triazole-1-yl)-2-(trimethylsilyloxy)propane

Product 1

HCID 9862025HCID 9862025, compoundYield 186.9%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

A mixture of 7.50 g (0.02 mol) of 2-(2,4-difluorophenyl)-1,3-bis(1,2,4-triazole-1-yl)-2-(trimethylsilyloxy)propane, 25 ml of methanol, 2 ml of water and 1.0 ml of concd. hydrochloric acid was stirred at 30° C. for 1 h. The reaction mixture was concentrated to a volume of 10 ml and after adding 50 ml of water the pH of the hot solution was adjusted to 8 with 10% aqueous sodium hydroxide. After cooling the precipitated crystals were filtered off, and dried at 40° C. until the weight was constant to yield 6.06 g (93.5%) of the title compound. M.p.: 139–140° C.

Workup

  1. concentrationThe reaction mixture was concentrated to a volume of 10 ml
  2. additionafter adding 50 ml of water the pH of the hot solution
  3. temperatureAfter cooling the precipitated crystals
  4. filtrationwere filtered off
  5. customdried at 40° C. until the weight

Sources & evidence

ORD record
ord-62a977a3af3043749e5018d7d27db422
Source dataset
uspto-grants-2006_08
Patent number
US07094904B2

Reaction notes

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