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Sodium Hydroxide → HCID 76219300、化合物

HRID 2408958
ノート
印刷プレビュー

反応式

HRID 2408958 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

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

生成物 1

HCID 76219300HCID 76219300、化合物収率 91%

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 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)−.

後処理

  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

出典と根拠

ORDレコード
ord-7620f5ec61c641edae40e795e5adc0f7
出典データセット
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08815879B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート