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

HRID 2421972노트

반응식

HRID 2421972 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-7287a543af424e5b99c45b779645383d
출처 데이터셋
uspto-grants-2011_06
특허 번호
US07960380B2

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