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1-Pyrrolidinamine → HCID 57970128, compound

HRID 1666611
Notes
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Reaction equation

HRID 1666611 reaction equation
Cl[C:2]1[CH:7]=[C:6](Cl)[CH:5]=[C:4]([CH3:9])[N+:3]=1[O-].Cl.[NH2:12][C@H:13]1[CH2:17][CH2:16][N:15]([C:18](=[O:31])[CH2:19][C:20]2[CH:25]=[CH:24][C:23]([O:26][C:27]([F:30])([F:29])[F:28])=[CH:22][CH:21]=2)[CH2:14]1.NN1CCCC1.[CH3:38][CH:39]1[CH2:44][CH2:43][NH:42][CH2:41][CH2:40]1.C(N(CC)C(C)C)(C)C>C(O)CCC>[CH3:38][CH:39]1[CH2:44][CH2:43][N:42]([C:6]2[CH:5]=[C:4]([CH3:9])[N:3]=[C:2]([NH:12][C@H:13]3[CH2:17][CH2:16][N:15]([C:18](=[O:31])[CH2:19][C:20]4[CH:21]=[CH:22][C:23]([O:26][C:27]([F:28])([F:29])[F:30])=[CH:24][CH:25]=4)[CH2:14]3)[CH:7]=2)[CH2:41][CH2:40]1
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

7

Reactant 5

HCID 279461-PyrrolidinamineHCID 693814-MethylpiperidineHCID 81531DiisopropylethylamineHCID 12504008HCID 12504008, compoundHCID 86636479(S)-1-(3-aminopyrrolidin-1-yl)-2-(4-trifluoromethoxyphenyl)ethanone mono hydrochloride

Product 1

HCID 57970128
HCID 57970128, compound
Yield 3%

Reagents, catalysts & solvents 1

HCID 2631-ButanolSolvent

Conditions

Temperature
110 °C

Procedure

In the same manner as in Example 13 (1), 1-((S)-3-(4-chloro-6-methyl-1-oxypyridin-2-ylamino)pyrrolidin-1-yl)-2-(4-trifluoromethoxyphenyl)ethanone (0.64 g) was obtained from 2,4-dichloro-6-methylpyridin-1-oxide (0.50 g) and 1-((S)-3-aminopyrrolidin-1-yl)-2-(4-trifluoromethoxyphenyl)ethanone mono hydrochloride (1.1 g). (2) A mixture of 1-((S)-3-(4-chloro-6-methyl-1-oxypyridin-2-ylamino)pyrrolidin-1-yl)-2-(4-trifluoromethoxyphenyl)ethanone (300 mg), 4-methylpiperidine (0.30 g), N,N-diisopropylethylamine (0.40 mL), and n-butanol (0.60 mL) was heated at 110° C. for 15 h. The mixture was cooled to room temperature, then the solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (NH silica gel, ethyl acetate−ethyl acetate/methanol=10:1) to obtain the title compound (40 mg) and 1-((S)-3-(4,6′-dimethyl-1′-oxy-3,4,5,6-tetrahydro-2H-[1,4′]bipyridinyl-2′-ylamino)pyrrolidin-1-yl)-2-(4-trifluoromethoxyphenyl)ethanone (200 mg). (3) 1-((S)-3-(4,6′-Dimethyl-1′-oxy-3,4,5,6-tetrahydro-2H-[1,4′]bipyridinyl-2′-ylamino)pyrrolidin-1-yl)-2-(4-trifluoromethoxyphenyl)ethanone (200 mg) was dissolved in methanol (6 mL), followed by addition of 10% Pd—C (200 mg), and the mixture stirred overnight at 40° C. under hydrogen atmosphere. The catalyst was removed by Celite filtration, then the filtrate was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (NH silica gel, chloroform/methanol=10:1) to obtain the title compound (64 mg).

Workup

  1. temperatureThe mixture was cooled to room temperature
  2. customthe solvent was evaporated under reduced pressure
  3. customthe residue was purified by silica gel column chromatography (NH silica gel, ethyl acetate−ethyl acetate/methanol=10:1)

Sources & evidence

ORD record
ord-7ab834c923084f9597ce6439b0571492
Source dataset
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08044068B2

Reaction notes

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