Potassium Carbonate → HCID 58433490、化合物

HRID 1798956ノート

反応式

HRID 1798956 の反応式
[C:1]1([C:7]2(NC)[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl[C:16]1[C:21]([Cl:22])=[CH:20][C:19]([C:23]([F:26])([F:25])[F:24])=[CH:18][N:17]=1.C(=O)([O-])[O-].[K+].[K+].[CH3:33][N:34]1C(=O)CCC1>>[Cl:22][C:21]1[C:16]([NH:34][CH2:33][C:7]2([C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12]2)=[N:17][CH:18]=[C:19]([C:23]([F:26])([F:25])[F:24])[CH:20]=1

参加物

5

反応物 4

HCID 11430Potassium CarbonateHCID 13387N-methyl-2-pyrrolidoneHCID 1122342,3-Dichloro-5-(trifluoromethyl)pyridineHCID 262910N-Methyl-1-phenylcyclohexanamine

生成物 1

HCID 58433490HCID 58433490、化合物

実験手順

was prepared from 475 mg of 1-phenyl-cyclohexyl-methylamine by reaction with 596 mg of 2,3-dichloro-5-trifluoromethyl-pyridine in the presence of 354 mg potassium carbonate in 2.5 ml of NMP at 80° C. for 1 hour. After dilution with 20 ml of water, the product was extracted with 30 ml of ethyl acetate and purified by chromatography on silica gel with the eluents dichloromethane:methanol=98:2 to obtain 469 mg g of a light yellow oil.

後処理

  1. extractionAfter dilution with 20 ml of water, the product was extracted with 30 ml of ethyl acetate
  2. custompurified by chromatography on silica gel with the eluents dichloromethane
  3. custommethanol=98:2 to obtain 469 mg g of a light yellow oil

出典と根拠

ORDレコード
ord-9bf982e80f6d48d8aa002d8d0c53d794
出典データセット
uspto-grants-2013_01
特許番号
US08344004B2

反応ノート

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