Methanol → HCID 28879848, 화합물

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[C:1]([C:3]1[CH:14]=[CH:13][C:6]([O:7][CH2:8][CH2:9][C:10]([OH:12])=[O:11])=[CH:5][CH:4]=1)#[N:2].S(Cl)(Cl)=O.[CH3:19]O>>[C:1]([C:3]1[CH:14]=[CH:13][C:6]([O:7][CH2:8][CH2:9][C:10]([O:12][CH3:19])=[O:11])=[CH:5][CH:4]=1)#[N:2]

참가 물질

반응물 3

HCID 887Methanol

HCID 24386Thionyl Chloride

HCID 108215343-(4-cyanophenoxy)propanoic Acid

생성물 1

HCID 28879848HCID 28879848, 화합물수율 79%

실험 절차

A solution of 3.80 g (19.9 mmol) of 3-(4-cyanophenoxy)propanoic acid in 10 ml of methanol is cooled by an ice bath. 3 ml (40 mmol) of thionyl chloride are added drop by drop and then the reaction medium is agitated with solvent reflux for 2 hours. The reaction mixture is then concentrated under reduced pressure and the evaporation residue is purified by silica column chromatography eluting with the help of a dichloromethane/methanol mixture (99/1; v/v). The expected product is obtained in the form of a white solid with a yield of 79%.

후처리

temperaturereflux for 2 hours
concentrationThe reaction mixture is then concentrated under reduced pressure
customthe evaporation residue is purified by silica column chromatography
washeluting with the help of a dichloromethane/methanol mixture (99/1; v/v)

출처 및 근거

ORD 기록: ord-e07b5f85bb9342fbb34a13bb02cfdf27
출처 데이터셋: uspto-grants-2011_01
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US07872021B2

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