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N-[4-(2-Chloro-phenyl)-pyridin-3-yl]-2,2-dimethyl-propionamide → 4-(2-Chlorophenyl)pyridin-3-amine

HRID 1017440
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HRID 1017440 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[CH:13]=[CH:12][N:11]=[CH:10][C:9]=1[NH:14]C(=O)C(C)(C)C>Cl>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[CH:13]=[CH:12][N:11]=[CH:10][C:9]=1[NH2:14]
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참가 물질

3

반응물 1

HCID 18403361N-[4-(2-Chloro-phenyl)-pyridin-3-yl]-2,2-dimethyl-propionamide

생성물 1

HCID 184033604-(2-Chlorophenyl)pyridin-3-amine수율 95%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

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온도
92.5 °C

실험 절차

A suspension of 22.2 g (77 mmol) N-[4-(2-chloro-phenyl)-pyridin-3-yl]-2,2-dimethyl-propionamide in 730 ml 3 N hydrochloric acid solution was heated to 90-95° C. overnight. The reaction mixture was cooled to room temperature, washed with three 130 ml portions diethyl ether and 500 ml ethyl acetate were added. The aqueous phase was adjusted to pH 7-8 by addition of 28% sodium hydroxide solution under ice cooling. The organic phase was separated and the product was extracted with three 200 ml portions of ethyl acetate. The combined organic layers were dried (magnesium sulfate) and evaporated to give 14.9 g (95%) of the title compound as white crystals.

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. washwashed with three 130 ml portions diethyl ether and 500 ml ethyl acetate
  3. additionwere added
  4. additionThe aqueous phase was adjusted to pH 7-8 by addition of 28% sodium hydroxide solution under ice cooling
  5. customThe organic phase was separated
  6. extractionthe product was extracted with three 200 ml portions of ethyl acetate
  7. dry with materialThe combined organic layers were dried (magnesium sulfate)
  8. customevaporated

출처 및 근거

ORD 기록
ord-d3bae56760f74f5faeb9cdc2fafb308a
출처 데이터셋
uspto-grants-2002_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06479483B2

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