Dimethylformamide → 2-Chloro-5-nitronicotinic acid

HRID 1038452노트

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HRID 1038452 반응식
O[C:2]1[N:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].CN(C)C=O.S(Cl)([Cl:21])=O>>[Cl:21][C:2]1[N:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5]

참가 물질

4

반응물 3

HCID 6228DimethylformamideHCID 24386Thionyl ChlorideHCID 178524577HCID 178524577, 화합물

생성물 1

HCID 125426642-Chloro-5-nitronicotinic acid수율 68%

반응 조건

온도
80 °C

실험 절차

2-Hydroxy-5-nitro-nicotinic acid (2.7 mmol) in a mixture of N,N-dimethylformamide (2.7 mmol) and thionyl chloride (5 ml) was heated at 80° C. for 1 h. The mixture was allowed to cool and concentrated in vacuo. To the resulting residue was added ice-water (20 ml) and with vigorous stirring a precipitate formed. The precipitate was filtered off and dried in a vacuum oven to give a white solid (68%).

후처리

  1. temperatureto cool
  2. concentrationconcentrated in vacuo
  3. additionTo the resulting residue was added ice-water (20 ml)
  4. customformed
  5. filtrationThe precipitate was filtered off
  6. customdried in a vacuum oven

출처 및 근거

ORD 기록
ord-6db9494834d34011843b63404b3612a6
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08551990B2

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