Phosphorus oxychloride → 3,5-Dichloro-benzofuro[3,2-c]isoquinoline

반응식

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

참가 물질

반응물 2

HCID 24813Phosphorus oxychloride

HCID 1785169623-Chloro-benzofuro[3,2-c]isoquinoline-5-ol

생성물 1

HCID 867222733,5-Dichloro-benzofuro[3,2-c]isoquinoline

실험 절차

A mixture of 19B (11.8 mmol) in POCl3 (20 mL) was refluxed for 2 hours. After reaction completed, POCl3 was evaporated under reduced pressure. The residue was added into crushed ice and stirred for 10 min. The solids were collected by filtration and dried to give 3.2 g of a crude product, which was dissolved in dichloromethane and purified by flash chromatography (petroleum ether 1:1) and concentrated to give a pure product M19 (3.1 g).

후처리

temperaturewas refluxed for 2 hours
customAfter reaction
customPOCl3 was evaporated under reduced pressure
additionThe residue was added
custominto crushed ice
filtrationThe solids were collected by filtration
customdried

출처 및 근거

ORD 기록: ord-573149b925c84f3da98822107018f8eb
출처 데이터셋: uspto-grants-2015_03
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US08969373B2

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