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Hydrochloric Acid → HCID 59547222、化合物

HRID 1097199
ノート
印刷プレビュー

反応式

HRID 1097199 の反応式
[CH:1]([C:3]1[Se:7][C:6]([C:8]([O:10]C)=[O:9])=[CH:5][CH:4]=1)=[O:2].[OH-:12].[Na+].Cl>O.[N+]([O-])([O-])=O.[Ag+]>[Se:7]1[C:6]([C:8]([OH:10])=[O:9])=[CH:5][CH:4]=[C:3]1[C:1]([OH:2])=[O:12]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 59547225HCID 59547225、化合物

生成物 1

HCID 59547222HCID 59547222、化合物収率 80%

試薬・触媒・溶媒 2

HCID 24470Silver Nitrate触媒HCID 962Water溶媒3 回

実験手順

A solution of silver nitrate (6.26 g, 36.86 mmol) in water (10 mL) was added to methyl 5-formylselenophene-2-carboxylate (4.0 g, 18.43 mmol) at 0° C. for 5 min. Then a solution of sodium hydroxide (3.05 g, 76.34 mmol) in water (10 mL) was added to the reaction mixture at the same temperature for 5 min and stirred the mixture at room temperature (rt) for 1 h. The cooled reaction mixture was poured into ice cooled water and acidified with dil. HCl. The solution was extracted with ethyl acetate (3×100 mL) and the combined organic layer was washed with water, brine and dried over sodium sulfate. The solution was filtered and evaporated the solvent to give the product as off-white color solid (3.2 g, 80%), mp 293-295° C. 1H NMR (400 MHz, DMSO-d6): δ 13.48 (2H, br s, 2×—COOH), 7.82 (2H, s, H-3,4); LC-MS (negative ion mode): m/z 219, 217 (M−H)−.

後処理

  1. customThe cooled reaction mixture
  2. additionwas poured into ice
  3. extractionThe solution was extracted with ethyl acetate (3×100 mL)
  4. washthe combined organic layer was washed with water, brine
  5. dry with materialdried over sodium sulfate
  6. filtrationThe solution was filtered
  7. customevaporated the solvent

出典と根拠

ORDレコード
ord-e6ec22051b294e77880d87210a01a5e0
出典データセット
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08143237B2

反応ノート

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