Phosphorus oxychloride → HCID 21578662, 화합물

반응식

[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[NH:8][C:7](=O)[CH:6]=[C:5]2[C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([Cl:19])[CH:14]=1.P(Cl)(Cl)([Cl:22])=O>>[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[C:7]([Cl:22])[CH:6]=[C:5]2[C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([Cl:19])[CH:14]=1

참가 물질

반응물 2

HCID 24813Phosphorus oxychloride

HCID 12016671HCID 12016671, 화합물

생성물 1

HCID 21578662HCID 21578662, 화합물수율 100%

실험 절차

A mixture of intermediate (4) (0.16 mol) in phosphoryl chloride (500 ml) was stirred and refluxed for one night. The mixture was evaporated till dryness, the residue was taken up in ice and water, alkalized with NH4OH and extracted with DCM. The organic layer was decanted, dried (MgSO4), filtered off and evaporated, yielding 56 g (100%) 6-bromo-2-chloro-4-(3-chlorophenyl)quinoline, mp. 125° C. (intermediate 5).

후처리

temperaturerefluxed for one night
customThe mixture was evaporated till dryness
extractionextracted with DCM
customThe organic layer was decanted
dry with materialdried (MgSO4)
filtrationfiltered off
customevaporated

출처 및 근거

ORD 기록: ord-9b4dc5a241b04126ad43a26ab7064a83
출처 데이터셋: uspto-grants-2006_06
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US07067531B2

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