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Hydrochloric Acid → HCID 59547222, 화합물

HRID 1097199
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HRID 1097199 반응식
[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]
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참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 59547225HCID 59547225, 화합물

생성물 1

HCID 59547222HCID 59547222, 화합물수율 80%

시약·촉매·용매 2

HCID 24470Silver Nitrate촉매HCID 962Water용매3회

실험 절차

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)−.

후처리

  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

출처 및 근거

ORD 기록
ord-e6ec22051b294e77880d87210a01a5e0
출처 데이터셋
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08143237B2

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