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Methanol → Methyl 2-bromoisonicotinate hydrochloride

HRID 625211
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HRID 625211 반응식
[Br:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][N:10]=1)[C:5]([OH:7])=[O:6].S(Cl)([Cl:13])=O.[CH3:15]O>>[ClH:13].[Br:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][N:10]=1)[C:5]([O:7][CH3:15])=[O:6]
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참가 물질

4

반응물 3

HCID 887MethanolHCID 24386Thionyl ChlorideHCID 2227012-Bromoisonicotinic acid

생성물 1

HCID 86705927Methyl 2-bromoisonicotinate hydrochloride수율 80%

실험 절차

Into a 500-mL round bottom flask, was placed a solution of 2-bromoisonicotinic acid (10 g, 49.75 mmol, 1.00 equiv) in methanol (200 mL). This was followed by dropwise addition of thionyl chloride (24 g, 203.39 mmol, 4.09 equiv) with stirring at 0° C.-5° C. The resulting solution was stirred for 5 h at 70° C. in an oil bath. The resulting mixture was concentrated under vacuum, to yield 10 g (80%) of methyl 2-bromoisonicotinate hydrochloride as a white solid.

후처리

  1. customInto a 500-mL round bottom flask, was placed
  2. stirringThe resulting solution was stirred for 5 h at 70° C. in an oil bath
  3. concentrationThe resulting mixture was concentrated under vacuum

출처 및 근거

ORD 기록
ord-2020d52d38da4647af79a8cd2f8d224a
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09301951B2

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