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

HRID 972546노트

반응식

HRID 972546 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-2yl)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 1 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 2 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-4c9e8b88b26548829fa7efaf84f4b570
출처 데이터셋
uspto-grants-1977_10
특허 번호
US04053486

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