Ammonium Chloride → HCID 15422793, compound

HRID 2297359Notes

Reaction equation

HRID 2297359 reaction equation
[CH3:1][Mg]Cl.[CH3:4][Si:5]1([CH3:12])[CH2:10][CH2:9][C:8](=[O:11])[CH2:7][CH2:6]1.[Cl-].[NH4+]>O1CCCC1>[CH3:1][C:8]1([OH:11])[CH2:9][CH2:10][Si:5]([CH3:12])([CH3:4])[CH2:6][CH2:7]1

Participants

5

Reactant 3

HCID 25517Ammonium ChlorideHCID 5470171,1-dimethylsilinan-4-oneHCID 178418332HCID 178418332, compound

Product 1

HCID 15422793HCID 15422793, compoundYield 90%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

To a tetrahydrofuran solution of 1.0M methylmagnesium chloride under ice cooling was added dropwise 14.2 g of 4,4-dimethyl-4-silacyclohexanone (which is synthesized by the disclosure of JP-A 7-309878). After two hours of agitation, an aqueous solution of ammonium chloride was added for hydrolysis. After ordinary post-treatments including extraction, washing and concentration, the product was purified by sublimation, obtaining 14.2 g (yield 90%) of 1,4,4-trimethyl-4-silacyclohexanol.

Workup

  1. customis synthesized by the disclosure of JP-A 7-309878)
  2. extractionextraction
  3. washwashing
  4. concentrationconcentration
  5. customthe product was purified by sublimation

Sources & evidence

ORD record
ord-770f74deadeb43d8b74165cff1e6f6ce
Source dataset
uspto-grants-2002_12
Patent number
US06492089B2

Reaction notes

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