Pyridinium chloride → 6,7-Dichloro-1-benzothiophene-5-ol

반응식

[Cl:1][C:2]1[C:3]([O:12]C)=[CH:4][C:5]2[CH:9]=[CH:8][S:7][C:6]=2[C:10]=1[Cl:11].Cl.N1C=CC=CC=1>>[Cl:1][C:2]1[C:3]([OH:12])=[CH:4][C:5]2[CH:9]=[CH:8][S:7][C:6]=2[C:10]=1[Cl:11]

참가 물질

반응물 2

HCID 10176127Pyridinium chloride

HCID 132899966,7-Dichloro-5-methoxybenzo[b]thiophene

생성물 1

HCID 132899976,7-Dichloro-1-benzothiophene-5-ol수율 1%

실험 절차

A mixture of 45 g of 6,7-dichloro-5-methoxybenzo[b]thiophene and 5 g of pyridine hydrochloride is stirred at 180° for 1 hour. The mixture is cooled, triturated with water and extracted thrice with ether. The ether solution is washed with water, dried and concentrated to give 0.42 g of 6,7-dichloro-5-hydroxybenzo[b]thiophene as a tan-colored solid. Recrystallization from acetone-hexane gives prisms, mp 97°-98°.

후처리

temperatureThe mixture is cooled
customtriturated with water
extractionextracted thrice with ether
washThe ether solution is washed with water
customdried
concentrationconcentrated

출처 및 근거

ORD 기록: ord-0d9f1e079729447ea026f3a9f6b782e8
출처 데이터셋: uspto-grants-1985_07
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US04528399

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