Guanidine Hydrochloride → 4-(dimethoxymethyl)pyrimidin-2-amine

HRID 552113ノート

反応式

HRID 552113 の反応式
[CH3:1][O:2][CH:3]([O:7][CH3:8])N(C)C.[CH3:9][C:10]([CH:12](OC)OC)=O.[OH-].[Na+].Cl.[NH2:20][C:21]([NH2:23])=[NH:22]>O>[CH3:8][O:7][CH:3]([O:2][CH3:1])[C:12]1[CH:10]=[CH:9][N:22]=[C:21]([NH2:23])[N:20]=1

参加物

6

反応物 4

HCID 5742Guanidine HydrochlorideHCID 14798Sodium HydroxideHCID 78373Dimethylformamide dimethyl acetalHCID 80650Pyruvic aldehyde dimethyl acetal

生成物 1

HCID 49130324-(dimethoxymethyl)pyrimidin-2-amine収率 36.6%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

A solution of 5.5 mL (41 mmol, 1.0 eq.) of dimethylformamide dimethyl acetal and 5.0 mL (41 mmol, 1.0 eq.) pyruvic aldehyde dimethyl acetal was heated at 100° C. for 16 h. Methanol was removed in vacuo to afford a brown oil. A solution of 1.8 g (45 mmol, 1.1 eq.) of sodium hydroxide in 5 mL of water was added to a solution of 4.3 g (45 mmol, 1.1 eq.) of guanidine HCl in 10 mL of water. The resulting solution was added to the above described oil. The resulting mixture was stirred at room temperature for 48 h. The mixture was filtered to provide 2.5 g (15 mmol, 36%) of 2-aminopyrimidine-4-carboxaldehyde dimethylacetal (I-8).

後処理

  1. customMethanol was removed in vacuo
  2. customto afford a brown oil
  3. additionThe resulting solution was added to the
  4. filtrationThe mixture was filtered

出典と根拠

ORDレコード
ord-d31f6c9f1c634c039334b5fbae7ea635
出典データセット
uspto-grants-2011_05
特許番号
US07951803B2

反応ノート

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