Boron trifluoride etherate → Methyl 2-methyl-1,3-dithiolane-2-propanoate

HRID 235690

반응식

HRID 235690 반응식
[C:1]([O:8][CH3:9])(=[O:7])[CH2:2][CH2:3]C(C)=O.[CH:10]([SH:13])([SH:12])[CH3:11].B(F)(F)F.[CH3:18][CH2:19]OCC>CO>[CH3:11][C:10]1([CH2:3][CH2:2][C:1]([O:8][CH3:9])=[O:7])[S:13][CH2:19][CH2:18][S:12]1

참가 물질

5

반응물 3

HCID 8000Boron trifluoride etherate2회HCID 336451,1-EthanedithiolHCID 69354Methyl levulinate

생성물 1

HCID 10921676Methyl 2-methyl-1,3-dithiolane-2-propanoate

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Into a mixture of about 100 g of methyl levulinate and about 100 ml of ethanedithiol was slowly poured boron trifluoride etherate until reflux began. An about 500 ml portion of methanol was added followed by sufficient boron trifluoride etherate to make a total of about 100 ml of this reagent. The mixture was stirred overnight, the solvent removed and the residue poured into saturated sodium bi-carbonate. The mixture was extracted with ether. The ether extract was dried, the solvent removed and the residue distilled at about 97°-100° C., at about 0.55 mm, giving about 147 g of the desired title compound.

후처리

  1. temperatureuntil reflux
  2. customthe solvent removed
  3. additionthe residue poured into saturated sodium bi-carbonate
  4. extractionThe mixture was extracted with ether
  5. extractionThe ether extract
  6. customwas dried
  7. customthe solvent removed
  8. distillationthe residue distilled at about 97°-100° C., at about 0.55 mm

출처 및 근거

ORD 기록
ord-a6c17df02c8949b98cdcad08c60fd7ad
출처 데이터셋
uspto-grants-1987_02
특허 번호
US04640913

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