Iodoethane → HCID 14184042, compound

HRID 1073390Notes

Reaction equation

HRID 1073390 reaction equation
[CH3:1][C:2](CC)=O.C(=O)([O-])[O-].[K+].[K+].C(I)C.[OH:15][C:16]1[CH:17]=[C:18]2[C:23](=[CH:24][C:25]=1[O:26][CH3:27])[O:22][C:21]([CH3:29])([CH3:28])[CH2:20][C:19]2=[O:30]>>[CH2:1]([O:15][C:16]1[CH:17]=[C:18]2[C:23](=[CH:24][C:25]=1[O:26][CH3:27])[O:22][C:21]([CH3:28])([CH3:29])[CH2:20][C:19]2=[O:30])[CH3:2]

Participants

5

Reactant 4

HCID 6340IodoethaneHCID 6569Methyl Ethyl KetoneHCID 11430Potassium CarbonateHCID 12637720HCID 12637720, compound

Product 1

HCID 14184042HCID 14184042, compoundYield 95%

Procedure

In 100 ml of methyl-ethyl-ketone 4.45g (20 millimoles) of 6-hydroxy-7-methoxy-2,2-dimethy-4-chromanone are dissolved, whereupon 4.1 g (30 millimoles) of potassium carbonate and 4.7 g (2.4 ml, 30 millimoles) of ethyl iodide are added and the reaction mixture is refluxed for 5 hours. The precipitated inorganic salt is filtered off, washed twice with 20 ml of acetone each and the solvent is removed. The residue is crystallized from 90% ethanol. Thus 4.75 g of the desired compound are obtained, yield 95%. Mp.: 86°-87° C.

Workup

  1. additionare added
  2. temperaturethe reaction mixture is refluxed for 5 hours
  3. filtrationThe precipitated inorganic salt is filtered off
  4. washwashed twice with 20 ml of acetone each and the solvent
  5. customis removed
  6. customThe residue is crystallized from 90% ethanol

Sources & evidence

ORD record
ord-a175062ffcce4d188b94462c724ebb7b
Source dataset
uspto-grants-1990_11
Patent number
US04968819

Reaction notes

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