2-Methoxyethylamine → 6-(6-(2-methoxyethylamino)pyridin-3-yl)-1,3-dipropyl-1H-pyrrolo[3,2-d]pyrimidine-2,4(3H,5H)-dione

HRID 1801690ノート

反応式

HRID 1801690 の反応式
Cl[C:2]1[N:7]=[CH:6][C:5]([C:8]2[NH:16][C:15]3[C:14](=[O:17])[N:13]([CH2:18][CH2:19][CH3:20])[C:12](=[O:21])[N:11]([CH2:22][CH2:23][CH3:24])[C:10]=3[CH:9]=2)=[CH:4][CH:3]=1.[CH3:25][O:26][CH2:27][CH2:28][NH2:29]>CCO>[CH3:25][O:26][CH2:27][CH2:28][NH:29][C:2]1[N:7]=[CH:6][C:5]([C:8]2[NH:16][C:15]3[C:14](=[O:17])[N:13]([CH2:18][CH2:19][CH3:20])[C:12](=[O:21])[N:11]([CH2:22][CH2:23][CH3:24])[C:10]=3[CH:9]=2)=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 80182-MethoxyethylamineHCID 598566326-(6-chloropyridin-3-yl)-1,3-dipropyl-1H-pyrrolo[3,2-d]pyrimidine-2,4(3H,5H)-dione

生成物 1

HCID 598566356-(6-(2-methoxyethylamino)pyridin-3-yl)-1,3-dipropyl-1H-pyrrolo[3,2-d]pyrimidine-2,4(3H,5H)-dione収率 56.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
164 °C

実験手順

8a (100 mg) was suspended in methoxyethylamine (1.5 g), in EtOH (4 mL) in a pressure tube and stirred at 164° C. for 28 hrs. After cooling to room temperature, the solvent was removed and the solid was purified by column (26 g silica gel, RT Scientific) (CH2Cl2:MeOH=100:0 to 97:3). The fractions were evaporated and washed with ether to give the product 9a (63 mg). The mother liquid was evaporated and afforded another 30 mg of the product.

後処理

  1. temperatureAfter cooling to room temperature
  2. customthe solvent was removed
  3. customthe solid was purified by column (26 g silica gel, RT Scientific) (CH2Cl2:MeOH=100:0 to 97:3)
  4. customThe fractions were evaporated
  5. washwashed with ether

出典と根拠

ORDレコード
ord-93f254bf760147f0954078fa4a75616a
出典データセット
uspto-grants-2013_01
特許番号
US08349848B2

反応ノート

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