Dimethylformamide → HCID 13393784, 화합물

반응식

[OH:1][C:2]1[CH:11]=[CH:10][CH:9]=[C:8]2[C:3]=1[C:4](=O)[CH2:5][CH:6]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[O:7]2.P(Cl)(Cl)([Cl:21])=O.CN(C)[CH:26]=[O:27]>>[Cl:21][C:4]1[C:3]2[C:8](=[CH:9][CH:10]=[CH:11][C:2]=2[OH:1])[O:7][CH:6]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[C:5]=1[CH:26]=[O:27]

참가 물질

반응물 3

HCID 6228Dimethylformamide

HCID 24813Phosphorus oxychloride

HCID 5860905-Hydroxy-2-phenyl-4-chromanone

생성물 1

HCID 13393784HCID 13393784, 화합물

실험 절차

As in example 1, but using 2.4 g 5-hydroxy-flavanone, 20 ml dimethylformamide and 2.8 ml phosphorous oxychloride. Reaction time is forty hours at 75° C. After hydrolysis and usual work up the residual solid is purified by column chromatography. The best fractions are recrystallised in a mixture of toluene and hexane to give pure yellow crystalline 4-chloro-3-formyl-5-hydroxy-flav-3-ene; m.p. 165° C.

후처리

customReaction time
waitis forty hours at 75° C
customAfter hydrolysis and usual work up the residual solid
customis purified by column chromatography
customThe best fractions are recrystallised in a mixture of toluene and hexane

출처 및 근거

ORD 기록: ord-b7b8e3059cf34eca93d0f2a0df40fe93
출처 데이터셋: uspto-grants-1990_06
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US04935441

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