Methanol → 2-Furoylacetonitrile

HRID 568590ノート

反応式

HRID 568590 の反応式
C(O[C:4]([C:6]1[O:7][CH:8]=[CH:9][CH:10]=1)=[O:5])C.[H-].[Na+].[C:13](#[N:15])[CH3:14].CO>C1(C)C=CC=CC=1>[O:7]1[CH:8]=[CH:9][CH:10]=[C:6]1[C:4]([CH2:14][C:13]#[N:15])=[O:5]

参加物

6

反応物 4

HCID 887MethanolHCID 6342AcetonitrileHCID 11980Ethyl 2-furoateHCID 24758Sodium hydride

生成物 1

HCID 1416712-Furoylacetonitrile収率 76%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

63.05 grams (0.5 mole) of furan-2-carboxylic acid ethyl ester and 30.0 grams (1 mole) of sodium hydride (80 weight % suspension in white oil) were reacted with 41 grams (1 mole) of acetonitrile in 500 ml of toluene with the addition of 1 ml of methanol at 90° C. After 3 hours reaction time the toluene was distilled off, the residue stirred with 500 ml of water, acidified with hydrochloric acid to pH 1.5 and the precipitated product filtered off with suction and recrystallized from methanol. There were obtained 51.3 grams (76% of theory) of 2-furanoylacetonitrile having a melting point of 74°-75° C.

後処理

  1. distillationwas distilled off
  2. filtrationthe precipitated product filtered off with suction
  3. customrecrystallized from methanol

出典と根拠

ORDレコード
ord-8292bec4055745558c0380a92dd578d4
出典データセット
uspto-grants-1988_03
特許番号
US04728743

反応ノート

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