2,5-Dichlorophenol → 2,5-Dichloro-4-nitrophenol

HRID 1373747

反応式

HRID 1373747 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][C:3]=1[OH:9].[N+:10]([O-])([OH:12])=[O:11]>C(Cl)(Cl)(Cl)Cl>[Cl:1][C:2]1[CH:7]=[C:6]([N+:10]([O-:12])=[O:11])[C:5]([Cl:8])=[CH:4][C:3]=1[OH:9]

参加物

4

反応物 2

HCID 662,5-DichlorophenolHCID 944Nitric Acid

生成物 1

HCID 221082,5-Dichloro-4-nitrophenol収率 65.9%

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒2 回

実験手順

To a solution of 2,5-dichlorophenol (10 g, 61.3 mmol) in CCl4 (400 mL) at 0° C. was dropwise added 4.7 mL (73.6 mmol) of 70% HNO3 in 30 mL of CCl4 during 30 min. The reaction mixture was slowly warmed to room temperature and stirred for 1 hour. The yellow precipitate was collected by filtration and dried to give the desired product (8.4 g) at 62% yield. MS (DCI/NH3) m/z 224.91 (M+NH4)+; 1H NMR (500 MHz, DMSO-D6) δ ppm 7.17 (s, 1 H) 8.25 (s, 1 H) 12.12 (s, 1 H).

後処理

  1. customat 0° C.
  2. customduring 30 min
  3. filtrationThe yellow precipitate was collected by filtration
  4. customdried

出典と根拠

ORDレコード
ord-7145a40684404e4a9eb1af466e62e151
出典データセット
uspto-grants-2007_01
特許番号
US07163939B2

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