Methanol → 2-Furoylacetonitrile

HRID 568590노트

반응식

HRID 568590 반응식
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]

참가 물질

6

반응물 4

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

생성물 1

HCID 1416712-Furoylacetonitrile수율 76%

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-8292bec4055745558c0380a92dd578d4
출처 데이터셋
uspto-grants-1988_03
특허 번호
US04728743

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