Sodium Sulfate → HCID 10728422, compound

HRID 1781455Notes

Reaction equation

HRID 1781455 reaction equation
[CH:1]([C:4]1[CH:12]=[C:11]([CH:13]([CH3:15])[CH3:14])[CH:10]=[C:9]([CH:16]([CH3:18])[CH3:17])[C:5]=1[C:6](Cl)=[O:7])([CH3:3])[CH3:2].[H-].[Al+3].[Li+].[H-].[H-].[H-].[O-]S([O-])(=O)=O.[Na+].[Na+]>CCOCC>[CH:16]([C:9]1[CH:10]=[C:11]([CH:13]([CH3:15])[CH3:14])[CH:12]=[C:4]([CH:1]([CH3:3])[CH3:2])[C:5]=1[CH2:6][OH:7])([CH3:18])[CH3:17]

Participants

5

Reactant 3

HCID 24436Sodium SulfateHCID 926972,4,6-Triisopropylbenzoyl chlorideHCID 21226445Aluminium lithium hydride

Product 1

HCID 10728422HCID 10728422, compound

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent2×

Procedure

A solution of commercially available 2,4,6-triiso-propylbenzoyl chloride (35 g, 131.2 mmol) in 400 mL ether was added slowly to a suspension of lithium aluminum hydride (LAH) (4.89 g, 131.2 mmol) in ether (300 mL) at -15° C. The mixture was slowly warmed to room temperature over 18 hours. Saturated Na2SO4 solution was added slowly and the ether layer was separated, dried over MgSO4, and evaporated to dryness. The compound was used in the next step without further purification; NMR (CDCl3):δ1.2-1.4 (m, 18H), 2.8-3.0 (m, 1H), 3.3-3.5 (m, 2H), 4.8 (s, 2H), 7.1 (s, 2H) ppm.

Workup

  1. customthe ether layer was separated
  2. dry with materialdried over MgSO4
  3. customevaporated to dryness
  4. customThe compound was used in the next step without further purification

Sources & evidence

ORD record
ord-bce51b72e30d439bbb1868b775a9fdee
Source dataset
uspto-grants-1997_05
Patent number
US05633287

Reaction notes

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