Hydroxylamine, O-ethyl- → HCID 178449929, compound

HRID 1589101Notes

Reaction equation

HRID 1589101 reaction equation
[C:1]([CH:6]1[C:11](=[O:12])[CH:10]([C:13]([O:15][CH3:16])=[O:14])[CH:9]([C:17]2[C:22]([CH3:24])([CH3:23])[CH2:21][CH2:20][CH2:19][C:18]=2[CH3:25])[CH2:8][C:7]1=[O:26])(=O)[CH2:2][CH2:3][CH3:4].[CH2:27]([O:29][NH2:30])[CH3:28]>C(O)C>[CH2:27]([O:29][NH:30][C:1](=[C:6]1[C:11](=[O:12])[CH:10]([C:13]([O:15][CH3:16])=[O:14])[CH:9]([C:17]2[C:22]([CH3:23])([CH3:24])[CH2:21][CH2:20][CH2:19][C:18]=2[CH3:25])[CH2:8][C:7]1=[O:26])[CH2:2][CH2:3][CH3:4])[CH3:28]

Participants

4

Reactant 2

HCID 69357Hydroxylamine, O-ethyl-HCID 13044542HCID 13044542, compound

Product 1

HCID 178449929HCID 178449929, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

9.0 parts by weight of 2-butyryl-4-carbomethoxy-5-(1,3,3-trimethylcyclohex-1-en-2-yl)-cyclohexane-1,3-dione are dissolved in 100 parts by volume of ethanol, and 1.5 parts by weight of ethoxyamine are added. The mixture is stirred at room temperature for 8 hours and concentrated under reduced pressure. The residue is taken up in 50 parts by volume of methylene chloride and the solution is washed with 5% strength hydrochloric acid and water and concentrated under reduced pressure. 2-(1-Ethoxyaminobutylidene)-4-carbomethoxy-5-(1,3,3-trimethylcyclohex-1-en-2-yl)-cyclohexane-1,3-dione is obtained in quantitative yield, as crystals of melting point 70° C. (active ingredient No.3).

Workup

  1. additionare added
  2. concentrationconcentrated under reduced pressure
  3. washthe solution is washed with 5% strength hydrochloric acid and water
  4. concentrationconcentrated under reduced pressure

Sources & evidence

ORD record
ord-cc2d44d66ae34459a8c838a54abc3091
Source dataset
uspto-grants-1986_02
Patent number
US04568383

Reaction notes

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