Benzyl Alcohol → 6-(Phenylmethoxy)-9H-purin-2-amine

HRID 458297

反応式

HRID 458297 の反応式
[NH2:1][C:2]1[N:10]=[C:9]2[C:5]([NH:6][CH:7]=[N:8]2)=[C:4](Cl)[N:3]=1.[OH-].[Na+].[CH2:14]([OH:21])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1>>[NH2:1][C:2]1[N:10]=[C:9]2[C:5]([NH:6][CH:7]=[N:8]2)=[C:4]([O:21][CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[N:3]=1

参加物

4

反応物 3

HCID 244Benzyl AlcoholHCID 14798Sodium HydroxideHCID 53603492-Amino-6-chloropurine

生成物 1

HCID 45786-(Phenylmethoxy)-9H-purin-2-amine

反応条件

温度
100 °C

実験手順

To a 500 mL 3 neck round bottom flask equipped with a magnetic stirrer, temperature probe and nitrogen inlet was added 2-amino-6-chloropurine (20 g), sodium hyroxide (28 g) and benzyl alcohol (200 mL). The mixture was stirred for 20 minutes and then heated at 100° C. for 2–3 hours. The reaction mixture was then cooled to room temperature and partitioned between methyl t-butyl ether (300 mL) and water (300 mL). The aqueous layer was separated and the pH was adjusted to 7–8 with 6 M HCl. The resulting solid was filtered, washed with water (50 mL) and dried under vacuum at 50° C. for 20 hours to provide the desired product as a pale yellow solid (24.3 g).

後処理

  1. temperatureThe reaction mixture was then cooled to room temperature
  2. custompartitioned between methyl t-butyl ether (300 mL) and water (300 mL)
  3. customThe aqueous layer was separated
  4. filtrationThe resulting solid was filtered
  5. washwashed with water (50 mL)
  6. customdried under vacuum at 50° C. for 20 hours

出典と根拠

ORDレコード
ord-00228ee92a4f40cf830b6553a46cef50
出典データセット
uspto-grants-2007_03
特許番号
US07189849B2

関連ノート

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