Sodium Bicarbonate → HCID 178449933, compound

HRID 1906696Notes

Reaction equation

HRID 1906696 reaction equation
[C:1]([CH:6]1[C:11](=[O:12])[CH2:10][CH:9]([CH:13]2[CH2:19][CH2:18][O:17][CH:16]([CH:20]([CH3:22])[CH3:21])[O:15][CH2:14]2)[CH2:8][C:7]1=[O:23])(=O)[CH2:2][CH2:3][CH3:4].[Cl-].[CH2:25]([O:27][NH3+:28])[CH3:26].C(=O)(O)[O-].[Na+]>CO>[CH2:25]([O:27][NH:28][C:1](=[C:6]1[C:11](=[O:12])[CH2:10][CH:9]([CH:13]2[CH2:19][CH2:18][O:17][CH:16]([CH:20]([CH3:22])[CH3:21])[O:15][CH2:14]2)[CH2:8][C:7]1=[O:23])[CH2:2][CH2:3][CH3:4])[CH3:26]

Participants

5

Reactant 3

HCID 516892Sodium BicarbonateHCID 13473084HCID 13473084, compoundHCID 19001768HCID 19001768, compound

Product 1

HCID 178449933HCID 178449933, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

6.5 parts by weight of 2-butyryl-5-(2-isopropyl-1,3-dioxepan-5-yl)-cyclohexane-1,3-dione, 2.1 parts by weight of ethoxyammonium chloride and 1.8 parts by weight of sodium bicarbonate in 80 parts by volume of methanol are stirred for 16 hours at room temperature. The solvent is distilled off under reduced pressure, the residue is stirred with 50 parts by volume of water and 50 parts by volume of dichloromethane, the organic phase is separated off, the aqueous phase is extracted once with 50 parts by volume of dichloromethane, the combined organic phases are dried over sodium sulfate, and the solvent is distilled off under reduced pressure. 6.2 parts by weight of 2-(1-ethoxyamino-n-butylidene)-5-(2-isopropyl1,3-dioxepan-5-yl)-cyclohexane-1,3-dione are obtained as an oil (active ingredient No. 1).

Workup

  1. distillationThe solvent is distilled off under reduced pressure
  2. customthe organic phase is separated off
  3. extractionthe aqueous phase is extracted once with 50 parts by volume of dichloromethane
  4. dry with materialthe combined organic phases are dried over sodium sulfate
  5. distillationthe solvent is distilled off under reduced pressure

Sources & evidence

ORD record
ord-efad078866f64c24ab5a3d1d248f69ab
Source dataset
uspto-grants-1987_03
Patent number
US04654073

Reaction notes

Loading…