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Water → 4-Hydroxy-2,2,5,5-tetramethylhexan-3-one

HRID 2367863
ノート
印刷プレビュー

反応式

HRID 2367863 の反応式
[OH-:1].[Na+].Br[CH:4]([C:11]([CH3:14])([CH3:13])[CH3:12])[C:5](=[O:10])[C:6]([CH3:9])([CH3:8])[CH3:7].O>C(N(CC)C=O)C>[OH:1][CH:4]([C:11]([CH3:14])([CH3:13])[CH3:12])[C:5](=[O:10])[C:6]([CH3:9])([CH3:8])[CH3:7]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 12387514HCID 12387514、化合物

生成物 1

HCID 2195934-Hydroxy-2,2,5,5-tetramethylhexan-3-one

試薬・触媒・溶媒 1

HCID 12051Diethylformamide溶媒

反応条件

温度
110 °C

実験手順

5 g (0.125 mol) of sodium hydroxide powder was added to 11.6 g (0.05 mol) of 4-Bromo-2,2,5,5-tetramethyl-3-hexanone in 10 g of dry diethylformamide. This reaction mixture was heated to 110° C. for 2 hours, cooled to room temperature and 600 mL of water and 200 mL of hexanes added. The hexane layer was collected and the aqueous layer was washed three times with 50 ml of additional hexanes. The hexanes fractions were then combined, washed three times with 50 ml water, then dried with MgSO4. The product was collected as a crystalline solid after hexanes removal by atmospheric distillation.

後処理

  1. temperaturecooled to room temperature
  2. customThe hexane layer was collected
  3. washthe aqueous layer was washed three times with 50 ml of additional hexanes
  4. washwashed three times with 50 ml water
  5. dry with materialdried with MgSO4
  6. customThe product was collected as a crystalline solid
  7. customafter hexanes removal
  8. distillationby atmospheric distillation

出典と根拠

ORDレコード
ord-7eb41d6cf5a5401d96dfbf4d712ac80c
出典データセット
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08703103B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート