Tetrahydrofuran → 5-(2-Methyl-1,3-dioxolan-2-yl)-2-pentanone

HRID 972222노트

반응식

HRID 972222 반응식
[Li].[CH3:2][C:3]1([CH2:8][CH2:9][CH2:10][C:11]([OH:13])=O)[O:7][CH2:6][CH2:5][O:4]1.O1CCC[CH2:15]1.C[Li]>C(OCC)C>[CH3:2][C:3]1([CH2:8][CH2:9][CH2:10][C:11](=[O:13])[CH3:15])[O:4][CH2:5][CH2:6][O:7]1

참가 물질

6

반응물 4

HCID 8028TetrahydrofuranHCID 3028194LithiumHCID 13551185HCID 13551185, 화합물HCID 178418348HCID 178418348, 화합물

생성물 1

HCID 104196285-(2-Methyl-1,3-dioxolan-2-yl)-2-pentanone

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

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온도
0 °C

실험 절차

348 Mg. of the lithium salt of the ketal acid, 4-(2-methyl-1,3-dioxolan-2-yl)butanoic acid was dissolved in 5 ml. anhydrous tetrahydrofuran. The solution was cooled to 0° C and 1.25 ml. of a 1.6 molar solution of methyllithium in diethylether was added dropwise over a period of one hour while stirring under a nitrogen atmosphere. The solution was allowed to rise approximately to 20° C and kept at this temperature over a period of two hours. The reaction mixture was added to crushed ice and the organic solvents were removed in vacuo. The residue was extracted with ether, the extract was washed with a saturated sodium chloride solution, dried with magnesium sulfate, filtered and evaporated in vacuo to give crude 5-(2-methyl-1,3-dioxolan-2-yl)-2-pentanone.

후처리

  1. customto rise approximately to 20° C
  2. additionThe reaction mixture was added
  3. customto crushed ice
  4. customthe organic solvents were removed in vacuo
  5. extractionThe residue was extracted with ether
  6. washthe extract was washed with a saturated sodium chloride solution
  7. dry with materialdried with magnesium sulfate
  8. filtrationfiltered
  9. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-f1f584607a964a5388071f1aa251ec0c
출처 데이터셋
uspto-grants-1977_10
특허 번호
US04052413

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