Tert-butyl 4-(4-cyanophenyl)-3,6-dihydropyridine-1(2h)-carboxylate → Tert-butyl 4-(4-cyanophenyl)piperidine-1-carboxylate

HRID 541181ノート

反応式

HRID 541181 の反応式
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH2:14][CH2:13][N:12]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:11][CH:10]=2)=[CH:5][CH:4]=1)#[N:2]>C(OCC)(=O)C>[C:1]([C:3]1[CH:4]=[CH:5][C:6]([CH:9]2[CH2:10][CH2:11][N:12]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:13][CH2:14]2)=[CH:7][CH:8]=1)#[N:2]

参加物

3

反応物 1

HCID 11289112Tert-butyl 4-(4-cyanophenyl)-3,6-dihydropyridine-1(2h)-carboxylate2 回

生成物 1

HCID 22492960Tert-butyl 4-(4-cyanophenyl)piperidine-1-carboxylate収率 40%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

Around-bottom flask, containing a solution of tert-butyl 4-(4-cyanophenyl)-5,6-dihydropyridine-1(2H)-carboxylate (compound 1.3, 500 mg, 1.76 mmol, 1.00 equiv) in ethyl acetate (20 mL) was purged with nitrogen gas. To the solution was then added palladium on carbon (0.1 g, 10%, 60% water) and the flask was then further purged with nitrogen. The atmosphere was then changed to hydrogen and the mixture was stirred overnight at room temperature. After purging the system with nitrogen, the solids were removed by filtration and the filtrate was concentrated under reduced pressure to yield 0.2 g (40%) of the title compound as a yellow oil.

後処理

  1. customwas purged with nitrogen gas
  2. customadded palladium on carbon (0.1 g, 10%, 60% water) and the flask was then further purged with nitrogen
  3. customAfter purging the system with nitrogen
  4. customthe solids were removed by filtration
  5. concentrationthe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-4e715233ceeb4f438add9eabb4fa59bb
出典データセット
uspto-grants-2014_10
特許番号
US08871790B2

反応ノート

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