Diethyl Ether → HCID 18447139, compound

HRID 1269993Notes

Reaction equation

HRID 1269993 reaction equation
[CH3:1][C:2]1[C:10]([O:11][C:12]2[CH:19]=[CH:18][C:15]([C:16]#[N:17])=[CH:14][CH:13]=2)=[CH:9][CH:8]=[C:7]2[C:3]=1[CH:4]=[N:5][N:6]2C1CCCCO1.[ClH:26].O1CCOCC1.C(OCC)C>O1CCOCC1>[ClH:26].[CH3:1][C:2]1[C:10]([O:11][C:12]2[CH:19]=[CH:18][C:15]([C:16]#[N:17])=[CH:14][CH:13]=2)=[CH:9][CH:8]=[C:7]2[C:3]=1[CH:4]=[N:5][NH:6]2

Participants

5

Reactant 3

HCID 3283Diethyl EtherHCID 204431481,4-Dioxane hydrochlorideHCID 69432306HCID 69432306, compound

Product 1

HCID 18447139HCID 18447139, compoundYield 83%

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Procedure

Under nitrogen, 4-[(4-methyl-1-tetrahydro-2H-pyran-2-yl-1H-indazol-5-yl)oxy]benzonitrile (338 mg, 1.01 mmol) was dissolved in 1,4-dioxane (6 ml), followed by adding thereto a 4N-hydrochloric acid/1,4-dioxane solution (6 ml), and the resulting mixture was stirred at room temperature for 23 hours. After diethyl ether (30 ml) was added thereto and stirred, the precipitate was collected by filtration, washed with diethyl ether and then dried under reduced pressure to obtain 4-[(4-methyl-1H-indazol-5-yl)oxy]benzonitrile monohydrochloride (239 mg, yield 83%).

Workup

  1. additionby adding
  2. filtrationthe precipitate was collected by filtration
  3. washwashed with diethyl ether
  4. customdried under reduced pressure

Sources & evidence

ORD record
ord-994cca7299d44516b0b5cf88e05e8ebb
Source dataset
uspto-grants-2007_04
Patent number
US07199147B2

Reaction notes

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