Methyl 2-furoate → Methyl tetrahydrofuran-2-carboxylate

HRID 258640

反応式

HRID 258640 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

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

Methyl furoate is dissolved in 180 ml. of methanol. Thereafter 1 g. of 5 percent palladium-on-charcoal is added. The mixture is then hydrogenated at 1 to 3 atmospheres. After 45 hr. 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-ee81f0d183514ad8abf5321d37e63409
出典データセット
uspto-grants-1977_07
特許番号
US04033989

関連ノート

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