Acetamidine monohydrochloride → HCID 178499609, 화합물

HRID 1728550노트

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HRID 1728550 반응식
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

참가 물질

5

반응물 3

HCID 67170Acetamidine monohydrochlorideHCID 10942334Sodium MethoxideHCID 45790110HCID 45790110, 화합물

생성물 1

HCID 178499609HCID 178499609, 화합물수율 68.8%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
90 °C

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-6f61294cbacb42278a95db4cc312bf4e
출처 데이터셋
uspto-grants-1994_07
특허 번호
US05328910

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