Hydrochloric Acid → 3-Ethoxy-3-cyclobutene-1,2-dione

반응식

C([O:3][C:4]1(OCC)[C:7](OCC)([O:8][CH2:9][CH3:10])[CH2:6][C:5]1=[O:14])C.Cl>>[CH2:9]([O:8][C:7]1[C:4](=[O:3])[C:5](=[O:14])[CH:6]=1)[CH3:10]

참가 물질

반응물 2

HCID 313Hydrochloric Acid

HCID 203263262,2,3,3-Tetraethoxycyclobutan-1-one

생성물 1

HCID 110946163-Ethoxy-3-cyclobutene-1,2-dione수율 30%

실험 절차

##STR7## 45 g of 2,2,3,3-tetraethoxycyclobutanone are stirred vigorously at 50° C in 4 normal aqueous HCl until the starting material is no longer detectable. The reaction solution is then extracted for 20 hours continuously with diethyl ether and the organic extracts are dried over MgSO4 and concentrated. Precipitated crystals of 1-hydroxycyclobutene-3,4-dione are filtered off sharply and the liquid residue is distilled at 110° C/0.1 Torr to yield 6.65 g (=30% of theory) of the desired 1-ethoxycyclobutene-3,4-dione of the above structure.

후처리

extractionThe reaction solution is then extracted for 20 hours continuously with diethyl ether
dry with materialthe organic extracts are dried over MgSO4
concentrationconcentrated
customPrecipitated crystals of 1-hydroxycyclobutene-3,4-dione
filtrationare filtered off sharply
distillationthe liquid residue is distilled at 110° C/0.1 Torr

출처 및 근거

ORD 기록: ord-196e75bb90e24370bbfbc5dcc3c35dfa
출처 데이터셋: uspto-grants-1978_05
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US04092146

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