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4-(Aminomethyl)cyclohexanecarboxylic acid → 4-[(4,5-Diphenylpyrimidin-2-ylamino)methyl]cyclohexanecarboxylic acid

HRID 2235001
ノート
印刷プレビュー

反応式

HRID 2235001 の反応式
C(=O)([O-])[O-].[Cs+].[Cs+].[NH2:7][CH2:8][CH:9]1[CH2:14][CH2:13][CH:12]([C:15]([OH:17])=[O:16])[CH2:11][CH2:10]1.Cl[C:19]1[N:24]=[C:23]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[C:22]([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)=[CH:21][N:20]=1>C1(C)C=CC=CC=1>[C:25]1([C:23]2[C:22]([C:31]3[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=3)=[CH:21][N:20]=[C:19]([NH:7][CH2:8][CH:9]3[CH2:10][CH2:11][CH:12]([C:15]([OH:17])=[O:16])[CH2:13][CH2:14]3)[N:24]=2)[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 55264-(Aminomethyl)cyclohexanecarboxylic acidHCID 10796Cesium carbonateHCID 126742762-Chloro-4,5-diphenylpyrimidine

生成物 1

HCID 236526954-[(4,5-Diphenylpyrimidin-2-ylamino)methyl]cyclohexanecarboxylic acid収率 62.2%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

550 mg (1.69 mmol) of cesium carbonate were added to a suspension of 133 mg (0.84 mmol) of 4-aminomethylcyclohexanecarboxylic acid in 5 ml of toluene, and the mixture was stirred at room temperature. After 30 minutes, 150 mg (0.56 mmol) of 2-chloro-4,5-diphenyl-pyrimidine were added, and the mixture was stirred at 120° C. for 31 hours. The solvent was removed in vacuo and the residue was mixed with dichloromethane and water. The resulting precipitate was filtered off with suction. 135 mg (62%) of the desired product were obtained.

後処理

  1. stirringthe mixture was stirred at 120° C. for 31 hours
  2. customThe solvent was removed in vacuo
  3. additionthe residue was mixed with dichloromethane and water
  4. filtrationThe resulting precipitate was filtered off with suction

出典と根拠

ORDレコード
ord-2c2c878a42fe493b989ccf7d23c40323
出典データセット
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07713988B2

反応ノート

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