Hydrochloric Acid → HCID 19425216, 화합물

HRID 1720423노트

반응식

HRID 1720423 반응식
[F:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([O:9][CH:10]2[CH2:14][CH2:13][CH2:12][CH2:11]2)=[CH:4][C:3]=1[N:15]1[C:20](=[O:21])C2CCCC(=C2)C1=O.[Cl:26][C:27]1[CH:32]=[CH:31][C:30]([C:33]([NH2:37])([CH3:36])[CH2:34][CH3:35])=[CH:29][CH:28]=1.CN1[CH2:44][CH2:43][O:42]CC1.Cl>C1C=CC=CC=1>[F:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([O:9][CH:10]2[CH2:14][CH2:13][CH2:12][CH2:11]2)=[CH:4][C:3]=1[NH:15][C:20](=[O:21])[C:6]1[CH2:7][CH2:2][CH2:3][CH2:4][C:44]=1[C:43]([NH:37][C:33]([C:30]1[CH:29]=[CH:28][C:27]([Cl:26])=[CH:32][CH:31]=1)([CH3:36])[CH2:34][CH3:35])=[O:42]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 79724-MethylmorpholineHCID 19425191N-(2-fluoro-4-chloro-5-cyclopentyloxyphenyl)-3,4,5,6-tetrahydroisophthalimideHCID 2020814587649-89-6

생성물 1

HCID 19425216HCID 19425216, 화합물수율 39.6%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

N-(2-Fluoro-4-chloro-5-cyclopentyloxyphenyl)-3,4,5,6-tetrahydroisophthalimide (1.00 g, 2.75 mmol), 1-(4-chlorophenyl)-1-methylpropylamine (0.760 g, 4.14 mmol), N-methylmorpholine (0.310 g, 3.06 mmol) and benzene (15 ml) as a solvent were placed into a round bottom flask (50 cc) and stirred overnight at room temperature. After completion of the reaction, the reaction mixture was poured into 2N hydrochloric acid (30 ml), and the mixture was extracted with ethyl acetate (30 ml×3 portions). After drying the organic layer over anhydrous magnesium sulfate, the drying agent was removed, and the solvent was distilled off under reduced pressure. The resulting crude product was recrystallized from ethyl acetate/acetone to obtain N-(2-fluoro-4-chloro-5-cyclopentyloxyphenyl)-N'-(1-(4-chlorophenyl)-1-methylpropyl}-3,4,5,6-tetrahydrophthalamide as white crystals (0.298 g, 19.8% yield).

후처리

  1. customAfter completion of the reaction
  2. extractionthe mixture was extracted with ethyl acetate (30 ml×3 portions)
  3. dry with materialAfter drying the organic layer over anhydrous magnesium sulfate
  4. customthe drying agent was removed
  5. distillationthe solvent was distilled off under reduced pressure
  6. customThe resulting crude product was recrystallized from ethyl acetate/acetone

출처 및 근거

ORD 기록
ord-f60ae1f14566439ab5e6d05bb7b0b608
출처 데이터셋
uspto-grants-1996_04
특허 번호
US05506190

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