Nitric Acid → 4-Fluoro-3-nitrobenzaldehyde

HRID 64051

반응식

HRID 64051 반응식
[N+:1]([O-:4])(O)=[O:2].[F:5][C:6]1[CH:13]=[CH:12][C:9]([CH:10]=[O:11])=[CH:8][CH:7]=1>S(=O)(=O)(O)O>[F:5][C:6]1[CH:13]=[CH:12][C:9]([CH:10]=[O:11])=[CH:8][C:7]=1[N+:1]([O-:4])=[O:2]

참가 물질

4

반응물 2

HCID 944Nitric AcidHCID 680234-Fluorobenzaldehyde

생성물 1

HCID 5981294-Fluoro-3-nitrobenzaldehyde수율 77%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

반응 조건

온도
5 °C

실험 절차

Nitration mixture (sulfuric acid 40 ml+nitric acid 5.5 ml) was added dropwise to 4-fluorobenzaldehyde (10 g, 80.57 mmol) at 0° C. and the mixture was stirred at 5° C. for 20 min and at RT for 1 h. The mixture was quenched by the addition of crushed ice. The precipitate formed was filtered and was washed repeatedly with water to give white solid. The solid was dried under vacuum to give the product in 77% yield (10.5 g). 1H NMR (300 MHz, CDCl3): δ 10.04 (s, 1H), 8.58 (dd, 1H), 8.22-8.18 (m, 1H), 7.5 (t, 1H).

후처리

  1. customThe mixture was quenched by the addition of crushed ice
  2. customThe precipitate formed
  3. filtrationwas filtered
  4. washwas washed repeatedly with water
  5. customto give white solid
  6. customThe solid was dried under vacuum
  7. customto give the product in 77% yield (10.5 g)

출처 및 근거

ORD 기록
ord-102b47a80918421a8aefdc9de808d131
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09447091B2

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