1,4-Dioxane → HCID 178479751, 화합물

반응식

[Cl:1][C:2]1[C:11]2[C:6](=[CH:7][C:8]3[O:14][CH2:13][O:12][C:9]=3[CH:10]=2)[N:5]=[CH:4][C:3]=1[C:15]([O:17]CC)=[O:16].[O:20]1CCOCC1>>[ClH:1].[OH:20][C:2]1[C:11]2[C:6](=[CH:7][C:8]3[O:14][CH2:13][O:12][C:9]=3[CH:10]=2)[N:5]=[CH:4][C:3]=1[C:15]([OH:17])=[O:16]

참가 물질

반응물 2

HCID 312751,4-Dioxane

HCID 8245791,3-Dioxolo(4,5-g)quinoline-7-carboxylic acid, 8-chloro-, ethyl ester

생성물 1

HCID 178479751HCID 178479751, 화합물

실험 절차

Ethyl 4-chloro-6,7-methylenedioxyquinoline-3-carboxylate (18.5 g, 66.2 mmol) was dissolved in dioxane (100 mL) and treated with 50 mL 5 NNaOH and heated at reflux for 2 hour. After this time the solution was concentrated on a rotary evaporator, cooled and extracted with dichloromethane (2×100 mL). The remaining aqueous solution was then acidified with concentrated HCl and the precipitate collected and dried to afford 7 g of crude 4-hydroxy-6,7-methylenedioxyquinoline-3-carboxylic acid hydrochloride.

후처리

temperatureheated
temperatureat reflux for 2 hour
concentrationAfter this time the solution was concentrated on a rotary evaporator
temperaturecooled
extractionextracted with dichloromethane (2×100 mL)
customthe precipitate collected
customdried

출처 및 근거

ORD 기록: ord-8f7fa91b84384c239207573cd35e246f
출처 데이터셋: uspto-grants-2006_05
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US07053104B2

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