Methylamine → 1,3-Propanediol, 2-[(2-amino-9H-purin-9-yl)methoxy]-

HRID 1252681ノート

反応式

HRID 1252681 の反応式
[NH2:1][C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][N:8]2[CH2:11][O:12][CH:13]([CH2:24][O:25]C(=O)C2C=CC=CC=2)[CH2:14][O:15]C(=O)C2C=CC=CC=2)=[CH:4][N:3]=1.CN>>[NH2:1][C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][N:8]2[CH2:11][O:12][CH:13]([CH2:14][OH:15])[CH2:24][OH:25])=[CH:4][N:3]=1

参加物

3

反応物 2

HCID 6329MethylamineHCID 137140202-Amino-9-[(2-benzoyloxy-1-(benzoyloxymethyl)ethoxy)methyl]-9H-purine

生成物 1

HCID 30100981,3-Propanediol, 2-[(2-amino-9H-purin-9-yl)methoxy]-

実験手順

A mixture of 0.844 g (1.88 mM) of 2-amino-9-[(2-benzoyloxyl-1-(benzoyloxymethyl)ethoxy)methyl]-9H-purine and 100 ml of a 40% aqueous methylamine solution was stirred at room temperature for 30 minutes. The mixture was flash evaporated to a yellow oil which was then washed with water. The aqueous layer was then extracted twice with methylene chloride. The aqueous layer containing the product was then flash evaporated to a light yellow oil. Recrystallization of the oil in hot acetonitrile yielded the title compound as an analytically pure ivory solid, mpt. 148°-151°.

後処理

  1. customevaporated to a yellow oil which
  2. washwas then washed with water
  3. extractionThe aqueous layer was then extracted twice with methylene chloride
  4. additionThe aqueous layer containing the product
  5. customflash evaporated to a light yellow oil
  6. customRecrystallization of the oil in hot acetonitrile

出典と根拠

ORDレコード
ord-7e1638f9fe01443a90d57795846ab7ab
出典データセット
uspto-grants-1988_05
特許番号
US04745119

反応ノート

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