Ethanol → (3-(((2-Amino-6-chloro-4-pyrimidinyl)amino)methyl)-3-oxetanyl)methanol

HRID 1421872ノート

反応式

HRID 1421872 の反応式
[NH2:1][CH2:2][C:3]1([CH2:7][OH:8])[CH2:6][O:5][CH2:4]1.[NH2:9][C:10]1[N:15]=[C:14](Cl)[CH:13]=[C:12]([Cl:17])[N:11]=1.C(O)C>C(N(CC)CC)C>[NH2:9][C:10]1[N:15]=[C:14]([NH:1][CH2:2][C:3]2([CH2:7][OH:8])[CH2:6][O:5][CH2:4]2)[CH:13]=[C:12]([Cl:17])[N:11]=1

参加物

5

反応物 3

HCID 702EthanolHCID 655222-Amino-4,6-dichloropyrimidineHCID 18706850[3-(Aminomethyl)oxetan-3-yl]methanol

生成物 1

HCID 385214(3-(((2-Amino-6-chloro-4-pyrimidinyl)amino)methyl)-3-oxetanyl)methanol収率 32.8%

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

A mixture of 3-aminomethyl-3-hydroxymethyloxetane (1.17 g, 0.01 mol), 2-amino-4,6-dichloropyrimidine (1.64 g, 0.01 mol), ethanol (40 ml) and triethylamine (4 ml) was refluxed for one day. The solvent was distilled away under reduced pressure and ethyl acetate was added to the residue. The mixture was washed with water and dried over anhydrous magnesium sulfate. The solvent was distilled away under reduced pressure and the residue was purified by silica gel column chromatography (chloroform:methanol=20:1, later 10:1) to give colorless prism crystals (0.8 g, 32.8%), m.p. 185-186° C. (acetone).

後処理

  1. temperaturewas refluxed for one day
  2. distillationThe solvent was distilled away under reduced pressure and ethyl acetate
  3. additionwas added to the residue
  4. washThe mixture was washed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationThe solvent was distilled away under reduced pressure
  7. customthe residue was purified by silica gel column chromatography (chloroform

出典と根拠

ORDレコード
ord-efe1ab6d86274af3afad69431d791d0c
出典データセット
uspto-grants-2000_06
特許番号
US06080750

反応ノート

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