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

HRID 1244673노트

반응식

HRID 1244673 반응식
[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]

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 12069505HCID 12069505, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-24e5b6f4a4904db7aefe4a881f56ccf0
출처 데이터셋
uspto-grants-2006_10
특허 번호
US07122570B2

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