Methanol → tert-Butyl [1-(6-methoxypyridazin-3-yl)piperidin-4-yl]carbamate

HRID 2239569노트

반응식

HRID 2239569 반응식
Cl[C:2]1[N:7]=[N:6][C:5]([N:8]2[CH2:13][CH2:12][CH:11]([NH:14][C:15](=[O:21])[O:16][C:17]([CH3:20])([CH3:19])[CH3:18])[CH2:10][CH2:9]2)=[CH:4][CH:3]=1.[Na].[CH3:23][OH:24]>O>[CH3:23][O:24][C:2]1[N:7]=[N:6][C:5]([N:8]2[CH2:13][CH2:12][CH:11]([NH:14][C:15](=[O:21])[O:16][C:17]([CH3:20])([CH3:19])[CH3:18])[CH2:10][CH2:9]2)=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 887Methanol2회HCID 5360545SodiumHCID 379672514-(Boc-amino)-1-(6-chloro-3-pyridazinyl)piperidine

생성물 1

HCID 86625870tert-Butyl [1-(6-methoxypyridazin-3-yl)piperidin-4-yl]carbamate수율 75%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
120 °C

실험 절차

tert-Butyl [1-(6-chloropyridazin-3-yl)piperidin-4-yl]carbamate (0.50 g, 1.60 mmol) was dissolved in dry MeOH (15 ml) and sodium metal (0.073 g, 3.20 mmol) dissolved in MeOH (5 ml) was added. The reaction mixture was heated at in a microwave reactor at 120° C. for 4 h. The mixture was diluted with water (500 ml) and extracted with EtOAc (200 ml). The organic phase was dried (Na2SO4), filtered and evaporated to yield the title compound (0.37 g, 75%).

후처리

  1. additionwas added
  2. extractionextracted with EtOAc (200 ml)
  3. dry with materialThe organic phase was dried (Na2SO4)
  4. filtrationfiltered
  5. customevaporated

출처 및 근거

ORD 기록
ord-9b4b65b1e53d469cbdc18486f5b9bfaf
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07723333B2

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