Nitric Acid → 3-Chloro-2,4-dimethylphenol

HRID 561912

反応式

HRID 561912 の反応式
[N+]([O-])(O)=O.C(O)C.[C:8](=[O:10])=O.[Cl:11][C:12]1[C:17](C)=[CH:16][CH:15]=[CH:14][C:13]=1[CH3:19]>>[Cl:11][C:12]1[C:17]([CH3:16])=[C:8]([OH:10])[CH:15]=[CH:14][C:13]=1[CH3:19]

参加物

4

反応物 3

HCID 944Nitric AcidHCID 328851-Chloro-2,6-dimethylbenzene2 回HCID 19604758Methanedione--ethanol (1/1)

生成物 1

HCID 179117503-Chloro-2,4-dimethylphenol

実験手順

Nitration of 2-chloro-m-xylene. Nitric acid (90%, 50 mL) was cooled to −35° C. (ethanol-dry ice bath). 2-Chloro-m-xylene (10 mL) was added dropwise over 1 h keeping the temperature between −30° C. and −35° C. The reaction mixture was poured onto ice, stirred for 10 min, precipitate formed was collected by filtration, washed with water, dried. The crude product was purified on SiO2 (50 g), hexane-EtOAc (0 to 2% v/v). The product—yellow solid, 12.8 g, as a mixture of 2-chloro-1,3-dimethyl-4-nitro-benzene and chloro-1,3-dimethyl-5-nitro-benzene (4:1).

後処理

  1. customthe temperature between −30° C. and −35° C
  2. additionThe reaction mixture was poured onto ice
  3. customprecipitate formed
  4. filtrationwas collected by filtration
  5. washwashed with water
  6. customdried
  7. customThe crude product was purified on SiO2 (50 g), hexane-EtOAc (0 to 2% v/v)
  8. additionThe product—yellow solid, 12.8 g, as a mixture of 2-chloro-1,3-dimethyl-4-nitro-benzene and chloro-1,3-dimethyl-5-nitro-benzene (4:1)

出典と根拠

ORDレコード
ord-10b0b45ef6574d769ce42d9b699d30be
出典データセット
uspto-grants-2011_11
特許番号
US08063225B2

関連ノート

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