Sodium Bicarbonate → HCID 66818134, 화합물

HRID 1754911노트

반응식

HRID 1754911 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]=[CH:10][N:11]=1)[C:6]([OH:8])=O.[C:12]([O:16][C:17]([N:19]1[CH2:24][CH2:23][C:22]([NH2:27])([C:25]#[N:26])[CH2:21][CH2:20]1)=[O:18])([CH3:15])([CH3:14])[CH3:13].C([O-])(O)=O.[Na+]>CCO>[C:12]([O:16][C:17]([N:19]1[CH2:20][CH2:21][C:22]([C:25]#[N:26])([NH:27][C:6]([C:5]2[CH:9]=[CH:10][N:11]=[C:3]([O:2][CH3:1])[CH:4]=2)=[O:8])[CH2:23][CH2:24]1)=[O:18])([CH3:15])([CH3:13])[CH3:14]

참가 물질

5

반응물 3

HCID 516892Sodium BicarbonateHCID 8199422-Methoxyisonicotinic AcidHCID 22091429tert-Butyl 4-amino-4-cyanopiperidine-1-carboxylate

생성물 1

HCID 66818134HCID 66818134, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

4-(4,6-Dimethoxy-1,3,5-triazin-2-yl)-4-methylmorpholinium chloride 2,7-hydrate (1.06 g, 3.26 mmol) was added to a solution of 2-methoxy-isonicotinic acid (500 mg, 3.26 mmol) and 4-amino-4-cyano-piperidine-1-carboxylic acid tert-butyl ester (669 mg, 2.97 mmol) in EtOH (8.0 ml) at room temperature, and the mixture was stirred for 46.5 hours. An aqueous NaHCO3 solution was added to the reaction mixture, followed by extraction with AcOEt three times. The organic layers were washed with saturated brine, and then dried over anhydrous sodium sulfate and concentrated under reduced pressure. The resulting residue was purified by column chromatography (CH2Cl2/MeOH=99:1 to 95:5) to give 4-cyano-4-[(2-methoxy-pyridine-4-carbonyl)-amino]-piperidine-1-carboxylic acid tert-butyl ester as a colorless form (901 mg, 84%).

후처리

  1. extractionfollowed by extraction with AcOEt three times
  2. washThe organic layers were washed with saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe resulting residue was purified by column chromatography (CH2Cl2/MeOH=99:1 to 95:5)

출처 및 근거

ORD 기록
ord-f3123588ecfb40d1b36e625842acfeb9
출처 데이터셋
uspto-grants-2015_10
특허 번호
US09169254B2

반응 노트

불러오는 중…