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

HRID 1017440
Notes
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Reaction equation

HRID 1017440 reaction equation
[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]
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

3

Reactant 1

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

Product 1

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

Reagents, catalysts & solvents 1

HCID 313Hydrochloric AcidSolvent

Conditions

Temperature
92.5 °C

Procedure

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.

Workup

  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

Sources & evidence

ORD record
ord-d3bae56760f74f5faeb9cdc2fafb308a
Source dataset
uspto-grants-2002_11
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US06479483B2

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes