Aluminum(III) Chloride → HCID 20284769, compound

HRID 127524Notes

Reaction equation

HRID 127524 reaction equation
[C:1]([CH2:3][CH:4]1[C:16]2[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[NH:9][C:8]=2[S:7][CH2:6][CH2:5]1)#[N:2].[H-].[Al+3].[Li+].[H-].[H-].[H-].[Cl-].[Al+3].[Cl-].[Cl-]>CCOCC>[NH2:2][CH2:1][CH2:3][CH:4]1[C:16]2[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[NH:9][C:8]=2[S:7][CH2:6][CH2:5]1

Participants

5

Reactant 3

HCID 6451240Aluminum(III) ChlorideHCID 20284787HCID 20284787, compoundHCID 21226445Aluminium lithium hydride

Product 1

HCID 20284769HCID 20284769, compoundYield 79.3%

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent2×

Procedure

A suspension of the product of the above (2) (1.40 g) in ether (40 ml) is added dropwise to a suspension of lithium aluminium hydride (467 mg) and aluminium chloride (1.63 g) in ether. The mixture is stirred at room temperature for 2.5 hours and extracted with ether-ethyl acetate after addition of an aqueous solution of sodium hydroxide. The extract is condensed. The residue is crystallized from ethyl acetate-methanol to give the title compound as white crystals (1.13 g) melting at 136°-138° C. Yield: 79%.

Workup

  1. extractionextracted with ether-ethyl acetate
  2. additionafter addition of an aqueous solution of sodium hydroxide
  3. customcondensed
  4. customThe residue is crystallized from ethyl acetate-methanol

Sources & evidence

ORD record
ord-7bd85dbbfd0643b8b590a19837f7ae78
Source dataset
uspto-grants-1981_03
Patent number
US04256640

Reaction notes

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