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2,4-Dichlorobenzylamine → N-[(2,4-dichlorophenyl)methyl]-1-(2,2-difluoroethyl)-3-methyl-2-oxo-4-imidazolidinecarboxamide

HRID 2081058
Notes
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Reaction equation

HRID 2081058 reaction equation
[F:1][CH:2]([F:14])[CH2:3][N:4]1[CH2:8][CH:7]([C:9]([OH:11])=O)[N:6]([CH3:12])[C:5]1=[O:13].O.ON1C2C=CC=CC=2N=N1.Cl.C(N=C=NCCCN(C)C)C.C(N1CCOCC1)C.[Cl:46][C:47]1[CH:52]=[C:51]([Cl:53])[CH:50]=[CH:49][C:48]=1[CH2:54][NH2:55]>ClCCl>[Cl:46][C:47]1[CH:52]=[C:51]([Cl:53])[CH:50]=[CH:49][C:48]=1[CH2:54][NH:55][C:9]([CH:7]1[CH2:8][N:4]([CH2:3][CH:2]([F:1])[F:14])[C:5](=[O:13])[N:6]1[CH3:12])=[O:11]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

7

Reactant 5

HCID 14852,4-DichlorobenzylamineHCID 7525EthylmorpholineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27960291-Hydroxybenzotriazole hydrateHCID 866402181-(2,2-Difluoroethyl)-3-methyl-2-oxo-4-imidazolidinecarboxylic acid

Product 1

HCID 25096213
N-[(2,4-dichlorophenyl)methyl]-1-(2,2-difluoroethyl)-3-methyl-2-oxo-4-imidazolidinecarboxamide
Yield 11.4%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent2×

Procedure

A mixture of 1-(2,2-difluoroethyl)-3-methyl-2-oxo-4-imidazolidinecarboxylic acid (125 mg, 0.6 mmol), 1-hydroxybenzotriazole hydrate (110 mg, 0.720 mmol), 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (138 mg, 0.720 mmol) and N-ethylmorpholine (0.305 ml, 2.400 mmol) in dichloromethane (5 ml) was stirred for 10 minutes. [(2,4-Dichlorophenyl)methyl]amine (106 mg, 0.600 mmol) was added and the solution was stirred at room temperature for 3 days. The reaction mixture was diluted with dichloromethane (10 ml), washed with saturated sodium hydrogen carbonate solution (10 ml), water (10 ml) and brine (10 ml). The organic phase was dried (magnesium sulphate) and evaporated. The residue was purified by the mass-directed automated HPLC. The fraction containing the desired product was evaporated and the residue was triturated with diethyl ether and dried to give N-[(2,4-dichlorophenyl)methyl]-1-(2,2-difluoroethyl)-3-methyl-2-oxo-4-imidazolidinecarboxamide (25 mg). LC/MS [M+H]+=366, retention time=2.09 minutes.

Workup

  1. stirringthe solution was stirred at room temperature for 3 days
  2. washwashed with saturated sodium hydrogen carbonate solution (10 ml), water (10 ml) and brine (10 ml)
  3. dry with materialThe organic phase was dried (magnesium sulphate)
  4. customevaporated
  5. customThe residue was purified by the
  6. additionThe fraction containing the desired product
  7. customwas evaporated
  8. customthe residue was triturated with diethyl ether
  9. customdried

Sources & evidence

ORD record
ord-fc1652065ec04542bd78b1eb398af3fa
Source dataset
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07932282B2

Reaction notes

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