Sodium Sulfate → HCID 10728422, compound

HRID 2396258Notes

Reaction equation

HRID 2396258 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-triisopropylbenzoyl chloride (35g, 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 etherlayer was separated, dried over MgSO4, and evaporated to dryness. The compound was used in the next step without further purification; NMR (CDCl3): δ 1.2-1.4 (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 etherlayer 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-ba97f10fd49e46249842a3dedb3a494f
Source dataset
uspto-grants-1996_02
Patent number
US05491172

Reaction notes

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