Water → 2-(2,4-difluorophenyl)-6,7-dihydro-5H-pyrrolo[1,2-a]imidazole

HRID 1929995

反応式

HRID 1929995 の反応式
Br[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([F:11])=[CH:7][C:6]=1[F:12])=O.Cl.[NH:14]=[C:15]1[CH2:19][CH2:18][CH2:17][NH:16]1.C([O-])([O-])=O.[Na+].[Na+].O>CN(C=O)C>[F:12][C:6]1[CH:7]=[C:8]([F:11])[CH:9]=[CH:10][C:5]=1[C:3]1[N:14]=[C:15]2[CH2:19][CH2:18][CH2:17][N:16]2[CH:2]=1

参加物

6

反応物 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 27741852-Bromo-2',4'-difluoroacetophenoneHCID 178479085HCID 178479085、化合物

生成物 1

HCID 579298552-(2,4-difluorophenyl)-6,7-dihydro-5H-pyrrolo[1,2-a]imidazole収率 100%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 2-bromo-1-(2,4-difluorophenyl)ethanone (7.05 g, 30.0 mmol, prepared using General Procedure A.1 from 1-(2,4-difluorophenyl)ethanone), 2-iminopyrrolidine hydrochloride (10.9 g, 90 mmol, prepared following the procedure in J. Med. Chem., 2002, 45, 999-1001) and Na2CO3 (21.1 g, 199 mmol) in DMF (30 mL) was stirred overnight at about 80° C. The reaction mixture was cooled to ambient temperature, poured into water, and extracted with EtOAc. The organics were dried over MgSO4, filtered and concentrated under reduced pressure to give the crude title compound (6.61 g, 100%): LC/MS (Table 1, Method a) Rt=2.72 min; MS m/z: 221.0 (M+H)+.

後処理

  1. customprepared
  2. extractionextracted with EtOAc
  3. dry with materialThe organics were dried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-caf4c93ec4ed4b12ae69a951dcf4ab1d
出典データセット
uspto-grants-2012_05
特許番号
US08188083B2

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