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Sodium Carbonate → 7-Benzyl-3-pentyl-3,7-dihydro-1H-purine-2,6-dione

HRID 600571
ノート
印刷プレビュー

反応式

HRID 600571 の反応式
[CH2:1]([N:8]1[C:16]2[C:15](=[O:17])[NH:14][C:13](=[O:18])[NH:12][C:11]=2[N:10]=[CH:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(=O)([O-])[O-].[Na+].[Na+].I[CH2:26][CH2:27][CH2:28][CH2:29][CH3:30]>CN(C=O)C.O.CCOC(C)=O>[CH2:1]([N:8]1[C:16]2[C:15](=[O:17])[NH:14][C:13](=[O:18])[N:12]([CH2:26][CH2:27][CH2:28][CH2:29][CH3:30])[C:11]=2[N:10]=[CH:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 10340Sodium CarbonateHCID 123351-IodopentaneHCID 125005077-Benzyl-1H-purine-2,6(3H,7H)-dione

生成物 1

HCID 598538537-Benzyl-3-pentyl-3,7-dihydro-1H-purine-2,6-dione収率 44%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide
溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
40 °C

実験手順

7-Benzyl-3,7-dihydro-1H-purine-2,6-dione (5.0 g, 21 mmol) was mixed with sodium carbonate (3.3 g, 31 mmol) and 1-iodopentane (4.0 mL, 31 mmol) in DMF (60 mL). After being stirred at 40° C. for 18 h, the reaction mixture was diluted with water and EtOAc. The aqueous layer was extracted with EtOAc twice. The combined organic layers were dried, filtered and concentrated. The resulting white solid was collected and dried in vacuum oven at 50° C. for 18 h to provide the desired product (2.84 g, 44% yield). LCMS calculated for C17H21N4O2 (M+H): 313.2. found: 313.2.

後処理

  1. extractionThe aqueous layer was extracted with EtOAc twice
  2. customThe combined organic layers were dried
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe resulting white solid was collected
  6. customdried in vacuum oven at 50° C. for 18 h

出典と根拠

ORDレコード
ord-eb4967d70d304161bb035b0f93a3e2cf
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07902205B2

反応ノート

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