Methyl 2-furoate → Methyl tetrahydrofuran-2-carboxylate

HRID 328914

反応式

HRID 328914 の反応式
[O:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]([O:8][CH3:9])=[O:7].[H][H]>[Pd].CO>[O:1]1[CH2:5][CH2:4][CH2:3][CH:2]1[C:6]([O:8][CH3:9])=[O:7]

参加物

5

反応物 2

HCID 11902Methyl 2-furoateHCID 178418361HCID 178418361、化合物

生成物 1

HCID 169922Methyl tetrahydrofuran-2-carboxylate収率 89.8%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

Methyl furoate (50.4 g.) is dissolved in 180 ml. of methanol. Thereafter 1 g. of 5 percent palladium-on-charcoal is added. This mixture is then hydrogenated at 1 to 3 atmospheres. After 45 hours 0.79 moles of hydrogen are consumed. The black mixture is then filtered through Celite using 50 ml. of methanol to wash the reaction flask and filter. Evaporation of the filtrate under reduced pressure at 40°-45° C. bath temperature yields 51 g. of a yellow oil which is thereafter distilled, collecting that fraction boiling at 32°-35° C. Thereby, methyl tetrahydrofuroate (46.7 g.) is prepared.

後処理

  1. filtrationThe black mixture is then filtered through Celite
  2. washof methanol to wash the reaction flask
  3. filtrationfilter
  4. customEvaporation of the filtrate under reduced pressure at 40°-45° C. bath temperature
  5. customyields 51 g
  6. distillationof a yellow oil which is thereafter distilled
  7. customcollecting that fraction boiling at 32°-35° C

出典と根拠

ORDレコード
ord-6a7068fa3e3549b0bb9e7dd859328fea
出典データセット
uspto-grants-1977_04
特許番号
US04018803

関連ノート

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