Dimethylformamide → HCID 18706853、化合物

HRID 1421875ノート

反応式

HRID 1421875 の反応式
[NH2:1][C:2]1[N:7]=[C:6]([NH:8][CH2:9][C:10]2([CH2:14][OH:15])[CH2:13][CH2:12][CH2:11]2)[CH:5]=[C:4]([Cl:16])[N:3]=1.[Cl:17]N1C(=O)CCC1=O.CN(C)C=O>C(OCC)(=O)C>[NH2:1][C:2]1[N:7]=[C:6]([NH:8][CH2:9][C:10]2([CH2:14][OH:15])[CH2:13][CH2:12][CH2:11]2)[C:5]([Cl:17])=[C:4]([Cl:16])[N:3]=1

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 31398ChlorosuccinimideHCID 385223HCID 385223、化合物

生成物 1

HCID 18706853HCID 18706853、化合物収率 54.2%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

To 2-amino-6-chloro-4-[[(1-hydroxymethyl-1-cyclobutyl)methyl]amino]pyrimidine (0.24 g, 2.0 mmol) were added N-chlorosuccinimide (0.27 g, 2.0 mmol) and dimethylformamide (1.5 ml), and the mixture was stirred at room temperature for 2 days. Ethyl acetate was added and 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=100:1) to give colorless prism crystals (0.3 g, 54.2%), m.p. 179-181° C. (acetone).

後処理

  1. washthe mixture was washed with water
  2. dry with materialdried over anhydrous magnesium sulfate
  3. distillationThe solvent was distilled away under reduced pressure
  4. customthe residue was purified by silica gel column chromatography (chloroform:methanol=100:1)

出典と根拠

ORDレコード
ord-225cb617e10e4cb4ba5b09eccd0edbd6
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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