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

HRID 2367863
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HRID 2367863 반응식
[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]
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참가 물질

5

반응물 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 12387514HCID 12387514, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 12051Diethylformamide용매

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온도
110 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7eb41d6cf5a5401d96dfbf4d712ac80c
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08703103B2

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