Hydrochloric Acid → Methyl 2-(3-amino-4-chlorophenyl)acetate

HRID 1244673ノート

反応式

HRID 1244673 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([O:11][CH3:12])=[O:10])=[CH:4][C:3]=1[N+:13]([O-])=O.Cl>CO.[Zn]>[NH2:13][C:3]1[CH:4]=[C:5]([CH2:8][C:9]([O:11][CH3:12])=[O:10])[CH:6]=[CH:7][C:2]=1[Cl:1]

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 12069505HCID 12069505、化合物

生成物 1

HCID 21920780Methyl 2-(3-amino-4-chlorophenyl)acetate収率 88.1%

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 887Methanol溶媒

実験手順

13.07 mmol (3.0 g) of methyl 4-chloro-3-nitrobenzeneacetate and 198.8 mmol (13.0 g) of Zn dust are refluxed in 500 ml of MeOH for 10 minutes. Then, 13 ml of concentrated HCl is added in drops under reflux and refluxed for another 30 minutes. The suspension is hot-filtered, the methanol is distilled off, and the residue is set at pH 14 with NaHCO3 solution. Extraction with ethyl acetate, drying with Na2SO4 and distillation of the solution yields 2.3 g of methyl 3-amino-4-chlorobenzeneacetate as a beige solid.

後処理

  1. temperatureunder reflux
  2. temperaturerefluxed for another 30 minutes
  3. filtrationThe suspension is hot-filtered
  4. distillationthe methanol is distilled off
  5. extractionExtraction with ethyl acetate
  6. dry with materialdrying with Na2SO4 and distillation of the solution

出典と根拠

ORDレコード
ord-24e5b6f4a4904db7aefe4a881f56ccf0
出典データセット
uspto-grants-2006_10
特許番号
US07122570B2

反応ノート

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