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Sodium Hydroxide → HCID 178510347, 화합물

HRID 570004
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HRID 570004 반응식
S(O)(O)(=O)=O.[C:6]([N:9]1[CH2:14][CH2:13][N:12]([CH2:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH2:11][CH2:10]1)(=[NH:8])[NH2:7].[OH-].[Na+].[C:24]([C:26](=[CH:32]OCC)[C:27](OCC)=[O:28])#[N:25]>C(O)C>[CH2:15]([N:12]1[CH2:13][CH2:14][N:9]([C:6]2[N:7]=[C:27]([OH:28])[C:26]([C:24]#[N:25])=[CH:32][N:8]=2)[CH2:10][CH2:11]1)[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 789432-Propenoic acid, 2-cyano-3-ethoxy-, ethyl esterHCID 27566524-Benzylpiperazine-1-carboxamidine hemisulfate

생성물 1

HCID 178510347HCID 178510347, 화합물수율 29.6%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Mixed were 26.8 g of 1-amidino-4-benzylpiperazine sulfate and 133 ml of a 3% ethanol solution of sodium hydroxide, followed by an addition of 17.0 g of ethyl 2-cyano-3-ethoxyacrylate. After being refluxed for 5 hours, the reaction mixture was allowed to cool down. After distilling off ethanol from the reaction mixture, the residue was added with water and ethyl acetate. The resultant mixture was shaken. Precipitated colorless crystals of 2-(4-benzylpiperazino)-5-cyano-4-hydroxypyrimidine were collected by filtration, washed with water and then dried, thereby obtaining 7.4 g of 2-(4-benzylpiperazino)-5-cyano-4-hydroxypyrimidine (yield: 25%).

후처리

  1. additionMixed
  2. temperatureAfter being refluxed for 5 hours
  3. temperatureto cool down
  4. distillationAfter distilling off ethanol from the reaction mixture
  5. additionthe residue was added with water and ethyl acetate
  6. customPrecipitated colorless crystals of 2-(4-benzylpiperazino)-5-cyano-4-hydroxypyrimidine
  7. filtrationwere collected by filtration
  8. washwashed with water
  9. customdried

출처 및 근거

ORD 기록
ord-4e0ed297503a4f58a12092ce9108aa74
출처 데이터셋
uspto-grants-1988_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04734418

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