反応 #3822741
関連文献 (1)
openreactiondata ↗doi:10.1039/C8SC04228D
反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-297d8a5ba83d44c7af19f4a768d76a36表示可能な構造データがありません
CCOC(=O)C(=O)CC(=O)C1=C(C=C(C=C1C)C)C製品情報
ethyl 2,4-dioxo-4-(2,4,6-trimethylphenyl)butanoate (CAS 203870-51-3) product identity, structure identifiers and related reaction data for chemical intermediate research and sourcing review.
想定用途
専門的研究・工業用途限定
データベース ID 14945000
安全上の注意
For professional research and industrial use only. Review the supplier safety data sheet before handling.
合成データ
12 反応 · 12 文献
反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-297d8a5ba83d44c7af19f4a768d76a36反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: N2O3 gas was slowly passed into a stirred solution of the product of step A (16.2 g) in 300 mL of ethanol until the disappearance of starting material was confirmed by TLC. N2O3 gas was generated by the dropwise addition of 12N aqueous HCl solution into an aqueous slurry of NaNO2. The solvent was removed from the mixture and 200 mL of water was added to the residue. The product was then extracted into ether. The ether extract was dried over Na2SO4 and evaporated to give 16.1 g of a semi-solid. The solvent was removed from the mixture and 200 mL of water was added to the residue The product was then extracted into ether The ether extract was dried over Na2SO4 evaporated
ソース ID: ord-2c0368633ec242138ca06c698cd783de反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a solution of 2′,4′,6′-trimethylacetophenone (15 g, 92.6 mmol) and diethyl oxalate (20 g, 139 mmol) in 500 mL of anhydrous toluene was cautiously added 7.4 g of NaH (60% dispersion in mineral oil). The reaction mixture was slowly heated to reflux under N2. It was refluxed for about 20 minutes, then cooled, poured into ice-cold aqueous HCl solution, and extracted with ether. The extracts were washed with brine, dried over Na2SO4, filtered through a short silica gel pad and concentrated to give 16.2 g of a red oil which was used in the next reaction without further purification. The reaction mixture was slowly heated to reflux under N2 It was refluxed for about 20 minutes cooled poured into ice-cold aqueous HCl solution extracted with ether The extracts were washed with brine dried over Na2SO4 filtered through a short silica gel pad concentrated
ソース ID: ord-74dee2c9f0fb4bda88ffcdf9d9e3abbb反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: N2O3 gas was slowly passed into a stirred solution of the product of step A (16.2 g) in 300 mL of ethanol until the disappearance of starting material was confirmed by TLC. N2O3 gas was generated by the dropwise addition of 12N aqueous HCl solution into an aqueous slurry of NaNO2. The solvent was removed from the mixture and 200 mL of water was added to the residue. The product was then extracted into ether. The ether extract was dried over Na2SO4 and evaporated to give 16.1 g of a semi-solid. The solvent was removed from the mixture and 200 mL of water was added to the residue The product was then extracted into ether The ether extract was dried over Na2SO4 evaporated
ソース ID: ord-2c0368633ec242138ca06c698cd783de反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: N2O3 gas was slowly passed into a stirred solution of the product of step A (16.2 g) in 300 mL of ethanol until the disappearance of starting material was confirmed by TLC. N2O3 gas was generated by the dropwise addition of 12N aqueous HCl solution into an aqueous slurry of NaNO2. The solvent was removed from the mixture and 200 mL of water was added to the residue. The product was then extracted into ether. The ether extract was dried over Na2SO4 and evaporated to give 16.1 g of a semi-solid. The solvent was removed from the mixture and 200 mL of water was added to the residue The product was then extracted into ether The ether extract was dried over Na2SO4 evaporated
ソース ID: ord-2c0368633ec242138ca06c698cd783de反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a solution of 2′,4′,6′-trimethylacetophenone (15 g, 92.6 mmol) and diethyl oxalate (20 g, 139 mmol) in 500 mL of anhydrous toluene was cautiously added 7.4 g of NaH (60% dispersion in mineral oil). The reaction mixture was slowly heated to reflux under N2. It was refluxed for about 20 minutes, then cooled, poured into ice-cold aqueous HCl solution, and extracted with ether. The extracts were washed with brine, dried over Na2SO4, filtered through a short silica gel pad and concentrated to give 16.2 g of a red oil which was used in the next reaction without further purification. The reaction mixture was slowly heated to reflux under N2 It was refluxed for about 20 minutes cooled poured into ice-cold aqueous HCl solution extracted with ether The extracts were washed with brine dried over Na2SO4 filtered through a short silica gel pad concentrated
ソース ID: ord-74dee2c9f0fb4bda88ffcdf9d9e3abbb反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a solution of 2′,4′,6′-trimethylacetophenone (15 g, 92.6 mmol) and diethyl oxalate (20 g, 139 mmol) in 500 mL of anhydrous toluene was cautiously added 7.4 g of NaH (60% dispersion in mineral oil). The reaction mixture was slowly heated to reflux under N2. It was refluxed for about 20 minutes, then cooled, poured into ice-cold aqueous HCl solution, and extracted with ether. The extracts were washed with brine, dried over Na2SO4, filtered through a short silica gel pad and concentrated to give 16.2 g of a red oil which was used in the next reaction without further purification. The reaction mixture was slowly heated to reflux under N2 It was refluxed for about 20 minutes cooled poured into ice-cold aqueous HCl solution extracted with ether The extracts were washed with brine dried over Na2SO4 filtered through a short silica gel pad concentrated
ソース ID: ord-74dee2c9f0fb4bda88ffcdf9d9e3abbb反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: N2O3 gas was slowly passed into a stirred solution of the product of step A (16.2 g) in 300 mL of ethanol until the disappearance of starting material was confirmed by TLC. N2O3 gas was generated by the dropwise addition of 12N aqueous HCl solution into an aqueous slurry of NaNO2. The solvent was removed from the mixture and 200 mL of water was added to the residue. The product was then extracted into ether. The ether extract was dried over Na2SO4 and evaporated to give 16.1 g of a semi-solid. The solvent was removed from the mixture and 200 mL of water was added to the residue The product was then extracted into ether The ether extract was dried over Na2SO4 evaporated
ソース ID: ord-d9ea025a9a0a4f688e80e240ea0b34ac反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a solution of 2', 4', 6'-trimethylacetophenone (15 g, 92.6 mmol) and diethyl oxalate (20 g, 139 mmol) in 500 mL of anhydrous toluene was cautiously added 7.4 g of NaH (60% dispersion in mineral oil). The reaction mixture was slowly heated to reflux under N2. It was refluxed for about 20 minutes, then cooled, poured into ice-cold aqueous HCl solution, and extracted with ether. The extracts were washed with brine, dried over Na2SO4, filtered through a short silica gel pad and concentrated to give 16.2 g of a red oil which was used in the next reaction without further purification. The reaction mixture was slowly heated to reflux under N2 It was refluxed for about 20 minutes cooled poured into ice-cold aqueous HCl solution extracted with ether The extracts were washed with brine dried over Na2SO4 filtered through a short silica gel pad concentrated
ソース ID: ord-54fc6a8a376c4fd9a41d798a9116e90e反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: N2O3 gas was slowly passed into a stirred solution of the product of step A (16.2 g) in 300 mL of ethanol until the disappearance of starting material was confirmed by TLC. N2O3 gas was generated by the dropwise addition of 12N aqueous HCl solution into an aqueous slurry of NaNO2. The solvent was removed from the mixture and 200 mL of water was added to the residue. The product was then extracted into ether. The ether extract was dried over Na2SO4 and evaporated to give 16.1 g of a semi-solid. The solvent was removed from the mixture and 200 mL of water was added to the residue The product was then extracted into ether The ether extract was dried over Na2SO4 evaporated
ソース ID: ord-d9ea025a9a0a4f688e80e240ea0b34ac反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a solution of 2', 4', 6'-trimethylacetophenone (15 g, 92.6 mmol) and diethyl oxalate (20 g, 139 mmol) in 500 mL of anhydrous toluene was cautiously added 7.4 g of NaH (60% dispersion in mineral oil). The reaction mixture was slowly heated to reflux under N2. It was refluxed for about 20 minutes, then cooled, poured into ice-cold aqueous HCl solution, and extracted with ether. The extracts were washed with brine, dried over Na2SO4, filtered through a short silica gel pad and concentrated to give 16.2 g of a red oil which was used in the next reaction without further purification. The reaction mixture was slowly heated to reflux under N2 It was refluxed for about 20 minutes cooled poured into ice-cold aqueous HCl solution extracted with ether The extracts were washed with brine dried over Na2SO4 filtered through a short silica gel pad concentrated
ソース ID: ord-54fc6a8a376c4fd9a41d798a9116e90e反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: N2O3 gas was slowly passed into a stirred solution of the product of step A (16.2 g) in 300 mL of ethanol until the disappearance of starting material was confirmed by TLC. N2O3 gas was generated by the dropwise addition of 12N aqueous HCl solution into an aqueous slurry of NaNO2. The solvent was removed from the mixture and 200 mL of water was added to the residue. The product was then extracted into ether. The ether extract was dried over Na2SO4 and evaporated to give 16.1 g of a semi-solid. The solvent was removed from the mixture and 200 mL of water was added to the residue The product was then extracted into ether The ether extract was dried over Na2SO4 evaporated
ソース ID: ord-d9ea025a9a0a4f688e80e240ea0b34acPubChem References
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