Acetic Acid → HCID 178517719, 화합물

HRID 1762101노트

반응식

HRID 1762101 반응식
[NH2:1][C:2]1[NH:6][N:5]=[C:4]([N:7]2[CH2:12][CH2:11][O:10][CH2:9][CH2:8]2)[N:3]=1.Cl.[CH2:14](N1CCC(C(OCC)=O)C(=O)C1)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.[C:33]([OH:36])(=O)[CH3:34].[N:37]1C=[CH:41][CH:40]=[CH:39][CH:38]=1>O.CC(C)=O>[CH2:14]([CH:39]1[C:40]2[CH2:41][N:6]3[NH:5][C:4]([N:7]4[CH2:8][CH2:9][O:10][CH2:11][CH2:12]4)=[N:3][C:2]3=[N:1][C:34]=2[C:33](=[O:36])[NH:37][CH2:38]1)[C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 1049Pyridine2회HCID 2723880Ethyl 1-benzyl-3-oxopiperidine-4-carboxylate hydrochlorideHCID 44173793-morpholin-4-yl-1H-1,2,4-triazol-5-amine

생성물 1

HCID 178517719HCID 178517719, 화합물수율 72%

시약·촉매·용매 2

HCID 180Acetone용매HCID 962Water용매

실험 절차

A mixture of 50.8 g (0.3 mole) of 5-amino-3-morpholino-1H-1,2,4-triazole, 89.3 g (0.3 mole) of 1-benzyl-4-carbethoxy-3-oxo-piperidine-hydrochloride and 220 ml of acetic acid is refluxed for 7 hours under stirring. The reaction mixture is allowed to stand overnight, the precipitate is filtered and washed with acetone. The product thus obtained is dissolved in a mixture of 400 ml of water and 100 ml of pyridine under heating to boiling for 15 minutes. The solution is allowed to stand for a day, the precipitated crystals are filtered and washed with acetone. The product thus obtained (83.9 g) is dissolved in 260 ml of hot pyridine, to the solution 1000 ml of acetone are added. The precipitated crystals are filtered and washed with acetone. Thus 78.9 g of the desired compound are obtained, yield 72%, m.p.: 315°-317° C.

후처리

  1. temperatureis refluxed for 7 hours
  2. filtrationthe precipitate is filtered
  3. washwashed with acetone
  4. customThe product thus obtained
  5. temperatureunder heating
  6. waitto boiling for 15 minutes
  7. waitto stand for a day
  8. filtrationthe precipitated crystals are filtered
  9. washwashed with acetone
  10. customThe product thus obtained (83.9 g)
  11. additionare added
  12. filtrationThe precipitated crystals are filtered
  13. washwashed with acetone

출처 및 근거

ORD 기록
ord-d442ff68ea8a4507bac7f54d43aa8b86
출처 데이터셋
uspto-grants-1989_05
특허 번호
US04831029

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