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

HRID 2081058
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HRID 2081058 반응식
[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]
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참가 물질

7

반응물 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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-fc1652065ec04542bd78b1eb398af3fa
출처 데이터셋
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07932282B2

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