Triethylamine → HCID 135782141, 화합물

HRID 1905631노트

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HRID 1905631 반응식
C([N:3]([CH2:6][CH3:7])CC)C.Cl.Cl.[CH2:10]([N:17]1[CH2:22][CH2:21][C:20]([NH2:26])([C:23](Cl)=[O:24])[CH2:19][CH2:18]1)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.C(N1CCC(N)(C(O)=O)CC1)[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1.[OH-].[Na+]>C(Cl)Cl.C(Cl)CCl>[CH3:31][C:32]1[C:33]2[CH:28]=[CH:29][CH:30]=[CH:7][C:6]=2[NH:3][C:23](=[O:24])[C:20]2([CH2:21][CH2:22][N:17]([CH2:10][C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)[CH2:18][CH2:19]2)[N:26]=1

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 14798Sodium HydroxideHCID 14803624-Amino-1-benzylpiperidine-4-carboxylic AcidHCID 88658736HCID 88658736, 화합물

생성물 1

HCID 135782141HCID 135782141, 화합물

시약·촉매·용매 2

HCID 111,2-Dichloroethane용매HCID 6344Dichloromethane용매

실험 절차

A solution of 12.2 g (0.12 mole) of triethylamine in 100 ml of methylene chloride is added dropwise to a mixture of 5.4 g (0.04 mole) of 2-aminocetophenone and 13.0 g (0.04 mole) of 1-benzyl-4-amino-4-piperidine-carboxylic acid chloride dihydrochloride (prepared from 9.4 g (0.04 mole) of 1-benzyl-4-amino-4-carboxypiperidine by reaction with excess phosphorus-V chloride in methylene chloride at 25° C.) in 400 ml of ethylene chloride at 0° C., while stirring and under an N2 atmosphere, and the mixture is stirred at 0° C. for 1 hour and finally at 25° C. for 2 hours. It is then poured onto ice, the pH is brought to 10 with sodium hydroxide solution and the reaction product is extracted with methylene chloride. For purification, the product is chromatographed on silica gel 60 (Merck), a methylene chloride/methanol mixture (10:1) being used as the eluting agent.

후처리

  1. stirringthe mixture is stirred at 0° C. for 1 hour and finally at 25° C. for 2 hours
  2. additionIt is then poured onto ice
  3. extractionthe reaction product is extracted with methylene chloride
  4. customFor purification
  5. customthe product is chromatographed on silica gel 60 (Merck)

출처 및 근거

ORD 기록
ord-d9f09585cac048b89ef6eed536373772
출처 데이터셋
uspto-grants-1987_03
특허 번호
US04647560

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