Water → HCID 178474703, compound

HRID 1493511Notes

Reaction equation

HRID 1493511 reaction equation
[C:1]([CH:4]1[C:9](=[O:10])[CH2:8][CH:7]([CH:11]([CH3:24])[CH2:12][S:13][C:14]2[CH:19]=[CH:18][C:17]([C:20]([F:23])([F:22])[F:21])=[CH:16][CH:15]=2)[CH2:6][C:5]1=[O:25])(=O)[CH3:2].Cl.[CH2:27]([O:29][NH2:30])[CH3:28].C(=O)([O-])[O-].[K+].[K+].O>CO>[CH2:27]([O:29][NH:30][C:1](=[C:4]1[C:9](=[O:10])[CH2:8][CH:7]([CH:11]([CH3:24])[CH2:12][S:13][C:14]2[CH:15]=[CH:16][C:17]([C:20]([F:21])([F:23])[F:22])=[CH:18][CH:19]=2)[CH2:6][C:5]1=[O:25])[CH3:2])[CH3:28]

Participants

6

Reactant 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 76850O-ethylhydroxylamine hydrochlorideHCID 15017466HCID 15017466, compound

Product 1

HCID 178474703HCID 178474703, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

0.4 Gram of 2-acetyl-5-[1-methyl-2-(4-trifluoromethylphenylthio)ethyl]cyclohexane-1,3-dione and 0.1 g of ethoxyamine hydrochloride were dissolved in 10 ml of methanol and 0.15 g of potassium carbonate was added to the resulting solution which was then refluxed for 3 hours. The reaction solution was poured into water and extracted with chloroform. After removing chloroform, the residue was purified by thin layer chromatography (eluent, hexane:ethyl acetate=5:1) to obtain 0.3 g of 2-(1-ethoxyaminoethylidene)-5-[1-methyl-2-(4-trifluoromethylphenylthio)ethyl]cyclohexane-1,3-dione.

Workup

  1. temperaturewas then refluxed for 3 hours
  2. extractionextracted with chloroform
  3. customAfter removing chloroform
  4. customthe residue was purified by thin layer chromatography (eluent, hexane:ethyl acetate=5:1)

Sources & evidence

ORD record
ord-c67fd57dc9844638839fac88018afb32
Source dataset
uspto-grants-1991_06
Patent number
US05021579

Reaction notes

Loading…