Sulfuric Acid → 1-Methylethyl (2E)-2-butenoate

반응식

[C:1]([OH:6])(=[O:5])/[CH:2]=[CH:3]/[CH3:4].[CH3:7][CH:8](O)[CH3:9].S(=O)(=O)(O)O>>[CH:8]([O:5][C:1](=[O:6])/[CH:2]=[CH:3]/[CH3:4])([CH3:9])[CH3:7]

참가 물질

반응물 3

HCID 1118Sulfuric Acid

HCID 3776Isopropanol

HCID 637090Crotonic Acid

생성물 1

HCID 53543591-Methylethyl (2E)-2-butenoate수율 76.3%

실험 절차

Crotonic acid (193.7 g, 2.25 mol) was dissolved in 2-propanol (860 mL, 11.25 mol) in a 2 L flask and then well stirred, after which sulfuric acid (24 mL, 0.45 mol) was slowly added in droplets to the mixture and refluxed and stirred for 48 hours or longer. The stirred mixture was cooled to room temperature, after which the obtained mixture was washed with distilled water (1000 mL), and the organic layer was separated, neutralized and subjected to atmospheric distillation (80° C.), thus obtaining 220 g (1.71 mol, yield 76.3%) of crotonic acid isopropyl ester.

후처리

temperaturerefluxed
stirringstirred for 48 hours or longer
washafter which the obtained mixture was washed with distilled water (1000 mL)
customthe organic layer was separated
distillationsubjected to atmospheric distillation (80° C.)

출처 및 근거

ORD 기록: ord-0db0de5db94641a48e202ca03664dc84
출처 데이터셋: uspto-grants-2015_03
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US08993694B2

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