Triethylamine → 5-butyl-2,2-dimethyl-1,3-dioxane-4,6-dione

HRID 2090587노트

반응식

HRID 2090587 반응식
[CH3:1][C:2]1([CH3:10])[O:9][C:7](=[O:8])[CH2:6][C:4](=[O:5])[O:3]1.C(N(CC)CC)C.[C:18](Cl)(=O)[CH2:19][CH2:20][CH3:21]>ClCCl>[CH2:18]([CH:6]1[C:7](=[O:8])[O:9][C:2]([CH3:10])([CH3:1])[O:3][C:4]1=[O:5])[CH2:19][CH2:20][CH3:21]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 8855Butyryl chlorideHCID 162492,2-Dimethyl-1,3-dioxane-4,6-dione

생성물 1

HCID 110634455-butyl-2,2-dimethyl-1,3-dioxane-4,6-dione

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Meldrum's acid (2,2-dimethyl-1,3-dioxane-4,6-dione, 6.15 g, 42.7 mmol) and triethyl amine (8.63 g, 85.4 mmol) were dissolved in dichloromethane (60 mL). Butyric acid chloride (4.99 g, 46.9 mmol) was added to the solution thus obtained dropwise while cooling with ice, followed by stirring at room temperature for about 12 hours. The reaction mixture was concentrated under reduced pressure, and then the resulting residue was subjected to extraction using ethyl acetate. The thus-obtained organic layer was washed with dilute hydrochloric acid and an aqueous saturated sodium chloride solution, dried over magnesium sulfate, and then concentrated under reduced pressure. The resulting residue was purified using silica gel chromatography (developing solvent: n-hexane/ethyl acetate=8/2) to obtain 5-butyl-2,2-dimethyl-1,3-dioxane-4,6-dione.

후처리

  1. customthus obtained dropwise
  2. temperaturewhile cooling with ice
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. extractionthe resulting residue was subjected to extraction
  5. washThe thus-obtained organic layer was washed with dilute hydrochloric acid
  6. dry with materialan aqueous saturated sodium chloride solution, dried over magnesium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customThe resulting residue was purified

출처 및 근거

ORD 기록
ord-1f349d7513544363acf154a38eb848ed
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08436210B2

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