Diethyl Malonate → HCID 178483102, 화합물

HRID 2419640노트

반응식

HRID 2419640 반응식
S(O)(O)(=O)=O.[CH3:6][N:7]([CH3:11])[C:8]([NH2:10])=[NH:9].C[O-].[Na+].C([O:17][C:18](=O)[CH2:19][C:20](OCC)=[O:21])C>CO>[CH3:6][N:7]([CH3:11])[C:8]1[N:10]=[C:18]([OH:17])[CH:19]=[C:20]([OH:21])[N:9]=1

참가 물질

5

반응물 3

HCID 7761Diethyl MalonateHCID 220673Guanidine, 1,1-dimethyl-, sulfateHCID 10942334Sodium Methoxide

생성물 1

HCID 178483102HCID 178483102, 화합물수율 96.7%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

136 g (0.5 mol) of N,N-dimethylguanidine sulphate were added to a solution of 162 g (3 mol) of sodium methylate in 1 l of methanol at 0° to 5° C. 160 g (1 mol) of malonic acid diethyl ester were then allowed to run in without cooling and the mixture was stirred for 24 hours at room temperature. The solvent was then distilled off in vacuo and the residue was dissolved in water. The solution was brought to approximately pH 5 by adding glacial acetic acid; it was then cooled to 0°-5° C and the product which had precipitated was filtered off. 75 g (48% of theory) of 2-dimethylamino-4,6-dihydroxypyrimidine were thus obtained in the form of a colorless powder of melting point > 300° C.

후처리

  1. temperaturewithout cooling
  2. distillationThe solvent was then distilled off in vacuo
  3. dissolutionthe residue was dissolved in water
  4. additionby adding glacial acetic acid
  5. temperatureit was then cooled to 0°-5° C
  6. customthe product which had precipitated
  7. filtrationwas filtered off

출처 및 근거

ORD 기록
ord-5fa7fbcd51f542c6b883cd0cfef7ea3e
출처 데이터셋
uspto-grants-1978_08
특허 번호
US04107301

반응 노트

불러오는 중…