Water → Ethyl beta-[[2-[[(3-nitrophenyl)carbonyl]amino]acetyl]amino]pyridine-3-propanoate

HRID 378130

반응식

HRID 378130 반응식
[N+:1]([C:4]1[CH:16]=[CH:15][C:7](C(=O)NCC(O)=O)=[CH:6][CH:5]=1)([O-:3])=[O:2].Cl.Cl.[NH2:19][CH:20]([C:27]1[CH:28]=[N:29][CH:30]=[CH:31][CH:32]=1)[CH2:21][C:22]([O:24][CH2:25][CH3:26])=[O:23].[C:33]([O-:36])([O-])=O.[K+].[K+].O.[CH3:40][N:41]([CH:43]=[O:44])C>CN(C1C=CN=CC=1)C.C([O-])(O)=O.[Na+]>[N+:1]([C:4]1[CH:5]=[C:6]([C:43]([NH:41][CH2:40][C:33]([NH:19][CH:20]([C:27]2[CH:28]=[N:29][CH:30]=[CH:31][CH:32]=2)[CH2:21][C:22]([O:24][CH2:25][CH3:26])=[O:23])=[O:36])=[O:44])[CH:7]=[CH:15][CH:16]=1)([O-:3])=[O:2]

참가 물질

8

반응물 5

HCID 962WaterHCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 175494-Nitrohippuric acidHCID 22608516Ethyl 3-amino-3-(pyridin-3-yl)propanoate dihydrochloride

생성물 1

HCID 22608595Ethyl beta-[[2-[[(3-nitrophenyl)carbonyl]amino]acetyl]amino]pyridine-3-propanoate

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 516892Sodium Bicarbonate용매

실험 절차

A solution of p-nitrohippuric acid (5.6 g) in DMF (25 ml) was treated with DSC (9.6 g) and a catalytic amount of DMAP. After 5 hours, a solution of ethyl 3-amino-3-(3-pyridyl)propanoate 2HCl (8 g) and K2CO3 (2 g) in saturated aqueous NaHCO3 (25 ml) was added. The reaction mixture was stirred overnight at room temperature. H2O (25 ml) was added and the mixture was filtered. The resulting solid was washed with H2O (25 ml), slurried with CH3CN (25 ml) and filtered. Ethyl β-[[2-[[[3-nitrophenyl)carbonyl]amino]acetyl]amino]pyridine-3-propanoate (6.5 g) was obtained as a white solid. MS was consistent with the desired product.

후처리

  1. filtrationthe mixture was filtered
  2. washThe resulting solid was washed with H2O (25 ml)
  3. filtrationfiltered

출처 및 근거

ORD 기록
ord-0e0771c53c214db587efd5f6a1196709
출처 데이터셋
uspto-grants-2000_02
특허 번호
US06028223

연결된 노트

불러오는 중…