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

HRID 2239569ノート

反応式

HRID 2239569 の反応式
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

参加物

5

反応物 3

HCID 887Methanol2 回HCID 5360545SodiumHCID 379672514-(Boc-amino)-1-(6-chloro-3-pyridazinyl)piperidine

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
120 °C

実験手順

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%).

後処理

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

出典と根拠

ORDレコード
ord-9b4b65b1e53d469cbdc18486f5b9bfaf
出典データセット
uspto-grants-2010_05
特許番号
US07723333B2

反応ノート

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