Hydrochloric Acid → HCID 19425216、化合物

HRID 1720423ノート

反応式

HRID 1720423 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 19425216HCID 19425216、化合物収率 39.6%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-f60ae1f14566439ab5e6d05bb7b0b608
出典データセット
uspto-grants-1996_04
特許番号
US05506190

反応ノート

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