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2-Methoxyethanol → HCID 18332788、化合物

HRID 2269147
ノート
印刷プレビュー

反応式

HRID 2269147 の反応式
[NH2:1][C:2]1[N:10]=[CH:9][N:8]=[C:7]2[C:3]=1[N:4]=[CH:5][N:6]2[CH2:11][C:12]1[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=1.[CH3:19][O:20][CH2:21][CH2:22][OH:23]>[Na]>[NH2:1][C:2]1[N:10]=[C:9]([O:23][CH2:22][CH2:21][O:20][CH3:19])[N:8]=[C:7]2[C:3]=1[N:4]=[CH:5][N:6]2[CH2:11][C:12]1[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=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

4

反応物 2

HCID 80192-MethoxyethanolHCID 114364636-Amino-9-(4-fluorobenzyl)purine

生成物 1

HCID 18332788HCID 18332788、化合物収率 95%

試薬・触媒・溶媒 1

HCID 5360545Sodium溶媒

反応条件

温度
20 °C

実験手順

6-Amino-9-(4-fluorobenzyl)purine (100 mg, 0.36 mmol) was dissolved in 30 ml of sodium 2-mehoxyethoxide in 2-methoxyethanol and the solution was heated at 20° C. for 3 hours. The reaction mixture was concentrated in vacuo to dryness and to the residue was added water. The mixture was extracted with chloroform and the organic layer was washed with water, dried on sodium sulfate and concentrated in vacuo to dryness. The residue was purified with silica gel chromatography (2% methanol/chloroform) to give the subject compound (109 mg, yield 95%).

後処理

  1. concentrationThe reaction mixture was concentrated in vacuo to dryness and to the residue
  2. additionwas added water
  3. extractionThe mixture was extracted with chloroform
  4. washthe organic layer was washed with water
  5. customdried on sodium sulfate
  6. concentrationconcentrated in vacuo to dryness
  7. customThe residue was purified with silica gel chromatography (2% methanol/chloroform)

出典と根拠

ORDレコード
ord-362e64275a76417da4b34e10cad399eb
出典データセット
uspto-grants-2001_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06329381B1

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート