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Sodium hydride → 2,6-Dichloro-9-((2-(trimethylsilyl)ethoxy)methyl)-9H-purine

HRID 1453578
ノート
印刷プレビュー

反応式

HRID 1453578 の反応式
[Cl:1][C:2]1[N:10]=[C:9]2[C:5]([NH:6][CH:7]=[N:8]2)=[C:4]([Cl:11])[N:3]=1.[H-].[Na+].Cl[CH2:15][O:16][CH2:17][CH2:18][Si:19]([CH3:22])([CH3:21])[CH3:20]>CN(C)C=O>[Cl:1][C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][N:8]2[CH2:15][O:16][CH2:17][CH2:18][Si:19]([CH3:22])([CH3:21])[CH3:20])=[C:4]([Cl:11])[N:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 27242712-Chloromethyl 2-(trimethylsilyl)ethyl etherHCID 53244122,6-Dichloropurine

生成物 1

HCID 582852322,6-Dichloro-9-((2-(trimethylsilyl)ethoxy)methyl)-9H-purine

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

945 mg of 2,6-dichloropurine, 15 ml of DMF (dimethylformamide) and 288 mg of NaH are mixed and left at ambient temperature for 2 hours. 1.06 ml of 2-chloromethoxyethyltrimethylsilane are then added. The mixture is stirred for 18 hours at ambient temperature. The DMF is evaporated off. The product is taken up in methylene chloride. Washing is carried out with a saturated sodium bicarbonate solution and then once with H2O and, finally, with a saturated NaCl solution. Drying over Na2SO4 and evaporation to dryness are carried out. Purification is carried out by chromatography on silica with a CHCl3-AcOEt: 5-5 mixture for eluent. 876 mg of expected product are obtained, in the form of a yellow-colored oil.

後処理

  1. customThe DMF is evaporated off
  2. washWashing
  3. dry with materialDrying over Na2SO4 and evaporation to dryness
  4. customPurification

出典と根拠

ORDレコード
ord-9dae688878cc4cd98e06386b3760b190
出典データセット
uspto-grants-2009_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07476670B2

反応ノート

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