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

HRID 235690

反応式

HRID 235690 の反応式
[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

参加物

5

反応物 3

HCID 8000Boron trifluoride etherate2 回HCID 336451,1-EthanedithiolHCID 69354Methyl levulinate

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a6c17df02c8949b98cdcad08c60fd7ad
出典データセット
uspto-grants-1987_02
特許番号
US04640913

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