1,3-Dimethyl-2-imidazolidinone → HCID 178511217, 화합물

HRID 1165296노트

반응식

HRID 1165296 반응식
[NH2:1][C:2]1[S:3][CH:4]=[C:5]([CH2:7][S:8][CH2:9][CH2:10][C:11]#[N:12])[N:6]=1.Cl.[C:14](C1C=CNN=1)(=[NH:16])[NH2:15].CN1CCN(C)C1=O>O>[NH:1]([C:2]1[S:3][CH:4]=[C:5]([CH2:7][S:8][CH2:9][CH2:10][C:11]#[N:12])[N:6]=1)[C:14]([NH2:16])=[NH:15]

참가 물질

5

반응물 3

HCID 66611,3-Dimethyl-2-imidazolidinoneHCID 12918379Famotidine Impurity 33HCID 178479321HCID 178479321, 화합물

생성물 1

HCID 178511217HCID 178511217, 화합물수율 38.5%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To 5 g of 3-(2-aminothiazol-4-ylmethylthio)propionitrile were added 11 g of amidinopyrazole hydrochloride and 15 ml of 1,3-dimethyl-2- imidazolidinone and the mixture was heated to 110°-120° C. for 4 hours. After cooling, 120 ml of water was added to the reaction mixture and then the product was extracted twice with 50 ml of ethyl acetate and washed. The aqueous layer thus formed was collected, added with 11 g of anhydrous potassium carbonate and 10 ml of isopropanol, the crystals thus formed were collected by filtration to provide 2.33 g of 3-(2-guanidinothiazol-4-ylmethylthio)propionitrile having a melting point of 127°-128° C.

후처리

  1. temperaturethe mixture was heated to 110°-120° C. for 4 hours
  2. temperatureAfter cooling
  3. extractionthe product was extracted twice with 50 ml of ethyl acetate
  4. washwashed
  5. customThe aqueous layer thus formed
  6. customwas collected
  7. additionadded with 11 g of anhydrous potassium carbonate and 10 ml of isopropanol
  8. customthe crystals thus formed
  9. filtrationwere collected by filtration

출처 및 근거

ORD 기록
ord-308e15272a5e4653ab66ba1aa8c86b14
출처 데이터셋
uspto-grants-1990_03
특허 번호
US04908454

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