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Ammonium formate → 1-[4-[4-[4-(4-Methoxybutoxy)phenyl]piperidin-1-yl]phenyl]piperazine

HRID 1816773
ノート
印刷プレビュー

反応式

HRID 1816773 の反応式
C(OC([N:11]1[CH2:16][CH2:15][N:14]([C:17]2[CH:22]=[CH:21][C:20]([N:23]3[CH2:28][CH:27]=[C:26]([C:29]4[CH:34]=[CH:33][C:32]([O:35][CH2:36][CH2:37][CH2:38][CH2:39][O:40][CH3:41])=[CH:31][CH:30]=4)[CH2:25][CH2:24]3)=[CH:19][CH:18]=2)[CH2:13][CH2:12]1)=O)C1C=CC=CC=1.C([O-])=O.[NH4+]>CO.O1CCOCC1.[Pd]>[CH3:41][O:40][CH2:39][CH2:38][CH2:37][CH2:36][O:35][C:32]1[CH:33]=[CH:34][C:29]([CH:26]2[CH2:27][CH2:28][N:23]([C:20]3[CH:19]=[CH:18][C:17]([N:14]4[CH2:15][CH2:16][NH:11][CH2:12][CH2:13]4)=[CH:22][CH:21]=3)[CH2:24][CH2:25]2)=[CH:30][CH:31]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 2723923Ammonium formateHCID 696777324-[4-[4-[4-(4-methoxybutoxy)phenyl]-3,6-dihydro-2H-pyridin-1-yl]phenyl]piperazine-1-carboxylic acid benzyl ester

生成物 1

HCID 224946411-[4-[4-[4-(4-Methoxybutoxy)phenyl]piperidin-1-yl]phenyl]piperazine収率 81.1%

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 887Methanol溶媒
HCID 312751,4-Dioxane溶媒

反応条件

温度
100 °C

実験手順

To a mixture of 4-[4-[4-[4-(4-methoxybutoxy)phenyl]-3,6-dihydro-2H-pyridin-1-yl]phenyl]piperazine-1-carboxylic acid benzyl ester (2.20 g) and ammonium formate (1.25 g) in 90% methanol (44 ml) and dioxane was added 10% palladium on carbon at room temperature. The reaction mixture was heated at 100° C. for 2 hours. After cooling, the reaction mixture was filtered and evaporated. Sodium hydrogen carbonate solution was added to the residue. And the resulting precipitate was collected by filtration, washed with water and dried under hi-vacuum to give 1-[4-[4-[4-(4-methoxybutoxy)phenyl]piperidin-1-yl]phenyl]piperazine (1.36 g).

後処理

  1. temperatureAfter cooling
  2. filtrationthe reaction mixture was filtered
  3. customevaporated
  4. additionSodium hydrogen carbonate solution was added to the residue
  5. filtrationAnd the resulting precipitate was collected by filtration
  6. washwashed with water
  7. customdried under hi-vacuum

出典と根拠

ORDレコード
ord-fbf4101dc8404ba9aa56b03d817d6072
出典データセット
uspto-grants-2005_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06884868B1

反応ノート

読み込み中…

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