Acetamidine monohydrochloride → HCID 178499609、化合物

HRID 1728550ノート

反応式

HRID 1728550 の反応式
C([C:3](CC)([C:13]([O-:15])=[O:14])[C:4](CC)([C:8]([O-:10])=O)[C:5]([O-:7])=O)C.Cl.[C:19]([NH2:22])(=[NH:21])[CH3:20].[CH3:23][O-].[Na+]>CO>[OH:7][C:5]1[C:4]([CH2:3][C:13]([O:15][CH3:23])=[O:14])=[C:8]([OH:10])[N:22]=[C:19]([CH3:20])[N:21]=1

参加物

5

反応物 3

HCID 67170Acetamidine monohydrochlorideHCID 10942334Sodium MethoxideHCID 45790110HCID 45790110、化合物

生成物 1

HCID 178499609HCID 178499609、化合物収率 68.8%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
90 °C

実験手順

A mixture of triethyl-1,1,2-ethanetricarboxylate (20ml, 87mM) and acetamidine hydrochloride (8.22g, 87mM) was added to a solution of sodium methoxide (9.4g, 174mM) in dry methanol (100ml). The mixture was heated at 90° C. for 15 hours. The solvent was evaporated and the residue dissolved in water (150ml). The pH of the solution was adjusted to pH6 using concentrated hydrochloric acid. The resultant precipitate was collected by filtration, washed with water and then acetone, to give 4,6-dihydroxy-2-methylpyrimidine-5-acetic acid, methyl ester as a white solid (11.85g, 68.8%), m.p. >270° C.; microanalysis, found: C,48.5; H, 5.1; N, 14.1%; C7HSN204 requires C, 48.3; H,5.1; N, 13.8%; NMR: NaOD; 2.45(3H, s, pyrimidine-CH3), 3.57(2H,s,CH2), 3.87(3H,s,OCH3).

後処理

  1. customThe solvent was evaporated
  2. dissolutionthe residue dissolved in water (150ml)
  3. filtrationThe resultant precipitate was collected by filtration
  4. washwashed with water

出典と根拠

ORDレコード
ord-6f61294cbacb42278a95db4cc312bf4e
出典データセット
uspto-grants-1994_07
特許番号
US05328910

反応ノート

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