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Sodium Hydroxide → HCID 76219300, 화합물

HRID 2408958
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HRID 2408958 반응식
[OH-:1].[Na+].[Cl:3][C:4]([C:8]([CH3:11])([CH3:10])[CH3:9])=[CH:5][CH:6]=[O:7]>O.[N+]([O-])([O-])=O.[Ag+]>[Cl:3][C:4]([C:8]([CH3:11])([CH3:10])[CH3:9])=[CH:5][C:6]([OH:1])=[O:7]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 540583463-Chloro-4,4-dimethylpent-2-enal

생성물 1

HCID 76219300HCID 76219300, 화합물수율 91%

시약·촉매·용매 2

HCID 24470Silver Nitrate촉매HCID 962Water용매3회

실험 절차

A solution of sodium hydroxide (1.09 g, 27.3 mmol) in water (10 mL) was added to a solution of silver nitrate (2.32 g, 13.65 mmol) in water (15 mL) at ice cold temperature for 15 min. 3-Chloro-4,4-dimethylpent-2-enal (1.0 g, 6.825 mmol) was added dropwise at the same temperature for 15 min. The reaction mixture was allowed to rt and stirred for 1 h. The reaction mixture was poured into ice cooled water and filtered through hyflowgel to remove black particles. The hyflowgel bed was washed with hot water and cooled. The solution was acidified with dil. HCl and the solution was extracted with chloroform (3×100 mL) and the combined organic layer was washed with brine and dried over sodium sulfate. The solution was filtered and evaporated the solvent to give the product a white color solid (1.0 g, 91%), mp 146-148° C. 1H NMR (400 MHz, CDCl3): δ 8.02 (1H, br s), 6.11 (1H, s), 1.24 (9H, s); LC-MS (negative ion mode): m/z 161, 163 (M−H)−.

후처리

  1. customwas allowed to rt
  2. additionThe reaction mixture was poured into ice
  3. filtrationfiltered through hyflowgel
  4. customto remove black particles
  5. washThe hyflowgel bed was washed with hot water
  6. temperaturecooled
  7. extractionthe solution was extracted with chloroform (3×100 mL)
  8. washthe combined organic layer was washed with brine
  9. dry with materialdried over sodium sulfate
  10. filtrationThe solution was filtered
  11. customevaporated the solvent

출처 및 근거

ORD 기록
ord-7620f5ec61c641edae40e795e5adc0f7
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08815879B2

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