Acetyl chloride → HCID 85766638, compound

HRID 399287Notes

Reaction equation

HRID 399287 reaction equation
[Sn:1]([Cl:3])[Cl:2].[C:4]([CH2:7][C:8](=[O:10])[CH3:9])(=O)[CH3:5].C([Cl:14])(=O)C>C(OCC)C>[CH3:5][C:4]([Sn:1]([Cl:14])([Cl:3])[Cl:2])=[CH:7][C:8](=[O:10])[CH3:9]

Participants

5

Reactant 3

HCID 6367Acetyl chlorideHCID 24479Stannous ChlorideHCID 31261Acetylacetone

Product 1

HCID 85766638HCID 85766638, compoundYield 57.1%

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent

Procedure

94.8 g (0.5 mol) of tin(II) chloride and 50 g (0.5 mol) of acetylacetone in 200 ml of diethyl ether were placed in a reactor at room temperature. 39.3 g (0.5 mol) of acetyl chloride were metered in over 15 min, the temperature rising to 36° C. After a postreaction time of 2 h at room temperature, the white crystals which had precipitated out were filtered off and washed twice with 50 ml of diethyl ether. After drying under vacuum, 88 g (57% of theory) of 1-methylbut-1-en-3-onyltin trichloride (Cl3Sn--C(CH3)=CH--CO--CH3) melting at 129°-130° C. were isolated.

Workup

  1. customwere metered in over 15 min
  2. customrising to 36° C
  3. customAfter a postreaction time of 2 h at room temperature, the white crystals which had precipitated out
  4. filtrationwere filtered off
  5. washwashed twice with 50 ml of diethyl ether
  6. customAfter drying under vacuum

Sources & evidence

ORD record
ord-39227660c4244ff189c0ade24806efa3
Source dataset
uspto-grants-1998_10
Patent number
US05817851

Reaction notes

Loading…