Potassium Carbonate → HCID 23084249、化合物

HRID 1162332ノート

反応式

HRID 1162332 の反応式
[CH3:1][C:2]1[NH:3][C:4]([CH3:22])=[C:5]([CH2:7][NH:8][CH:9]2[CH2:14][CH2:13][N:12]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:11][CH2:10]2)[N:6]=1.C1CCN2C(=NCCC2)CC1.[C:34](=O)([O-])[O-:35].[K+].[K+]>ClCCl>[CH3:1][C:2]1[N:6]2[C:34](=[O:35])[N:8]([CH:9]3[CH2:14][CH2:13][N:12]([C:15]([O:17][C:18]([CH3:19])([CH3:21])[CH3:20])=[O:16])[CH2:11][CH2:10]3)[CH2:7][C:5]2=[C:4]([CH3:22])[N:3]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 23138170tert-butyl 4-(((2,5-dimethyl-1H-imidazol-4-yl)methyl)amino)-1-piperidinecarboxylate

生成物 1

HCID 23084249HCID 23084249、化合物収率 97%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

tert-Butyl 4-(((2,5-dimethyl-1H-imidazol-4-yl)methyl)amino)-1-piperidinecarboxylate (8.0 g) obtained in Example 88a) was dissolved in dichloromethane (100 ml), DBU (3.6 ml) and N,N′-carbonyldiimidazole (3.9 g) were added thereto. The reaction solution was mixed for 15 hours, and then the reaction solution was poured into an aqueous potassium carbonate solution and extracted with chloroform. The extract was dried over anhydrous magnesium sulfate, the solvent was distilled off under reduced pressure, and then the residue was purified with silica gel column to obtain a pale yellow oily title compound (7.8 g, 97%).

後処理

  1. additionThe reaction solution was mixed for 15 hours
  2. extractionextracted with chloroform
  3. dry with materialThe extract was dried over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off under reduced pressure
  5. customthe residue was purified with silica gel column

出典と根拠

ORDレコード
ord-791240d623194cfd87356eb57f1a516e
出典データセット
uspto-grants-2010_10
特許番号
US07820673B2

反応ノート

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