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Potassium Carbonate → HCID 58306160、化合物

HRID 1044945
ノート
印刷プレビュー

反応式

HRID 1044945 の反応式
[CH3:1][CH:2]([O:4][C:5]1[NH:6][C:7]([NH2:16])=[C:8]2[C:12]([N:13]=1)=[N:11][C:10]([O:14][CH3:15])=[N:9]2)[CH3:3].C(=O)([O-])[O-].[K+].[K+].Br[CH2:24][CH2:25][CH2:26][CH2:27][CH:28]1[CH2:33][CH2:32][N:31]([C:34]([O:36][C:37]([CH3:40])([CH3:39])[CH3:38])=[O:35])[CH2:30][CH2:29]1>CN(C=O)C.ClCCl>[NH2:16][C:7]1[N:6]=[C:5]([O:4][CH:2]([CH3:1])[CH3:3])[N:13]=[C:12]2[C:8]=1[N:9]=[C:10]([O:14][CH3:15])[N:11]2[CH2:24][CH2:25][CH2:26][CH2:27][CH:28]1[CH2:29][CH2:30][N:31]([C:34]([O:36][C:37]([CH3:38])([CH3:40])[CH3:39])=[O:35])[CH2:32][CH2:33]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 10358619tert-Butyl 4-(4-bromobutyl)piperidine-1-carboxylateHCID 178494010HCID 178494010、化合物

生成物 1

HCID 58306160HCID 58306160、化合物収率 41.7%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒2 回
HCID 6344
Dichloromethane
溶媒

実験手順

To a solution of 2-[(1-methylethyl)oxy]-8-(methyloxy)-1H-purin-6-amine (37 mg, 0.166 mmol) in DMF (0.5 ml) was added potassium carbonate (55 mg, 0.398 mmol) followed by a solution of 1,1-dimethylethyl 4-(4-bromobutyl)-1-piperidinecarboxylate (58 mg, 0.181 mmol) in DMF (0.2 ml) and the mixture was stirred at room temperature for 72 hours. The mixture was diluted with dichloromethane (5 ml) and washed with water (5 ml). The layers were separated using a hydrophobic frit, the aqueous layer was extracted again with dichloromethane (5 ml) and the combined organic extracts were evaporated. The residue was dissolved in methanol (0.6 ml) and purified by MDAP (Method A). The appropriate fractions were combined and evaporated under a stream of nitrogen in a blowdown apparatus to give the title compound as a colourless gum (32 mg).

後処理

  1. washwashed with water (5 ml)
  2. customThe layers were separated
  3. extractionthe aqueous layer was extracted again with dichloromethane (5 ml)
  4. customthe combined organic extracts were evaporated
  5. dissolutionThe residue was dissolved in methanol (0.6 ml)
  6. custompurified by MDAP (Method A)
  7. customevaporated under a stream of nitrogen in a blowdown apparatus

出典と根拠

ORDレコード
ord-282046417d3d473884a9c69f4dcf45a9
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08563717B2

反応ノート

読み込み中…

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