Hydrochloric Acid → HCID 178474707, compound

HRID 1493508Notes

Reaction equation

HRID 1493508 reaction equation
[C:1]([CH:4]1[C:9](=[O:10])[CH2:8][CH:7]([CH2:11][CH2:12][S:13][C:14]2[CH:19]=[CH:18][C:17]([O:20][C:21]([F:24])([F:23])[F:22])=[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(N(CC)CC)C.Cl>C(O)C.O>[CH2:27]([O:29][NH:30][C:1](=[C:4]1[C:9](=[O:10])[CH2:8][CH:7]([CH2:11][CH2:12][S:13][C:14]2[CH:15]=[CH:16][C:17]([O:20][C:21]([F:22])([F:23])[F:24])=[CH:18][CH:19]=2)[CH2:6][C:5]1=[O:25])[CH3:2])[CH3:28]

Participants

7

Reactant 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 76850O-ethylhydroxylamine hydrochlorideHCID 15017463HCID 15017463, compound

Product 1

HCID 178474707HCID 178474707, compound

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 962WaterSolvent

Procedure

0.19 Gram of 2-acetyl-5-[2-(4-trifluoromethoxyphenylthio)ethyl]cyclohexane-1,3-dione was dissolved in 10 ml of ethanol, and 0.07 g of ethoxyamine hydrochloride and 0.06 g of triethylamine were added to the resulting solution which was then stirred overnight at room temperature. The reaction solution was poured into water, acidified with dilute hydrochloric acid and extracted with chloroform. Chloroform was removed and the residue was purified by thin layer chromatography (eluent, hexane:ethyl acetate=5:1) to obtain 0.12 g of 2-(1-ethoxyaminoethylidene)-5 -[2-(4-trifluoromethoxyphenylthio)ethyl]cyclohexane-1,3-dione.

Workup

  1. extractionextracted with chloroform
  2. customChloroform was removed
  3. customthe residue was purified by thin layer chromatography (eluent, hexane:ethyl acetate=5:1)

Sources & evidence

ORD record
ord-742db9bf1b9046b593d524fa224c403d
Source dataset
uspto-grants-1991_06
Patent number
US05021579

Reaction notes

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