Benzoic Acid → 3-Ethoxy-2,4-dioxa-bicyclo[3,2,0]heptane

반응식

[CH2:1]([O:3][CH:4]([OH:6])[OH:5])[CH3:2].C(O)(=O)[C:8]1[CH:13]=[CH:12][CH:11]=CC=1>>[CH2:1]([O:3][CH:4]1[O:6][CH:12]2[CH:11]([CH2:8][CH2:13]2)[O:5]1)[CH3:2]

참가 물질

반응물 2

HCID 243Benzoic Acid

HCID 5231668Orthoameisensaureathylester

생성물 1

HCID 202893363-Ethoxy-2,4-dioxa-bicyclo[3,2,0]heptane수율 1,013.7%

실험 절차

130.8 g (1.5 mols) of cyclobutane-cis-1,2-diol, 222.6 g (1.5 mols) of orthoformic acid ethyl ester and 15.0 g of benzoic acid are heated from 90° to 120° C. in the course of 3 hours. The ethanol which forms is distilled off continuously. Fractional distillation in vacuo gives 179.5 g (83%) of 3-ethoxy-2,4-dioxa-bicyclo[3,2,0]heptane (stereoisomer mixture), boiling point11 63°.

후처리

distillationThe ethanol which forms is distilled off continuously
distillationFractional distillation in vacuo

출처 및 근거

ORD 기록: ord-6204157f7e9142c19291ae2069e12e2c
출처 데이터셋: uspto-grants-1981_02
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US04252738

반응 노트

불러오는 중…