Triethylamine → Ethyl 4-aminopyrimidine-2-carboxylate

HRID 2286673노트

반응식

HRID 2286673 반응식
Cl[C:2](=[CH2:5])[C:3]#[N:4].Br.[CH2:7]([O:9][C:10]([C:12]([NH2:14])=[NH:13])=[O:11])[CH3:8].C(N(CC)CC)C>C(O)C>[NH2:4][C:3]1[CH:2]=[CH:5][N:14]=[C:12]([C:10]([O:9][CH2:7][CH3:8])=[O:11])[N:13]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 701982-ChloroacrylonitrileHCID 233168511-Ethoxycarbonylformamidine hydrobromide

생성물 1

HCID 13060222Ethyl 4-aminopyrimidine-2-carboxylate수율 57.5%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of 2-chloroacrylonitrile(437 mg) and 1-ethoxycarbonylformamidine hydrobromide (985 mg) in ethanol (5 ml) was added dropwise triethylamine (1.01 g) at 0° C. The reaction mixture was stirred for 4 hours at ambient temperature and evaporated to dryness. The residue was dissolved in a mixture of ethyl acetate and water, and extracted with ethyl acetate three times. The combined extracts were dried over anhydrous magnesium sulfate and evaporated to dryness. The residue was triturated with diethyl ether to give ethyl 4-aminopyrimidine-2-carboxylate (480 mg), which was recrystallized from a mixture of ethyl acetate and benzene, mp. 101°-104° C.

후처리

  1. customevaporated to dryness
  2. dissolutionThe residue was dissolved in a mixture of ethyl acetate and water
  3. extractionextracted with ethyl acetate three times
  4. dry with materialThe combined extracts were dried over anhydrous magnesium sulfate
  5. customevaporated to dryness
  6. customThe residue was triturated with diethyl ether

출처 및 근거

ORD 기록
ord-65919f36734d414f9dc68c1156a5c8d8
출처 데이터셋
uspto-grants-1981_05
특허 번호
US04267176

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