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Ammonia → HCID 20278960、化合物

HRID 1156319
ノート
印刷プレビュー

反応式

HRID 1156319 の反応式
[F:1][C:2]1[CH:19]=[CH:18][C:5]([C:6]([CH:8]2[CH2:13][CH2:12][N:11]([CH:14]([CH3:17])[C:15]#[N:16])[CH2:10][CH2:9]2)=[O:7])=[CH:4][CH:3]=1.N.[H][H]>[Ni].CO>[NH2:16][CH2:15][CH:14]([N:11]1[CH2:12][CH2:13][CH:8]([C:6]([C:5]2[CH:4]=[CH:3][C:2]([F:1])=[CH:19][CH:18]=2)=[O:7])[CH2:9][CH2:10]1)[CH3:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 222AmmoniaHCID 134765514-(4-Fluorobenzoyl)-alpha-methyl-1-piperidineacetonitrileHCID 178418361HCID 178418361、化合物

生成物 1

HCID 20278960HCID 20278960、化合物収率 100%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 887Methanol溶媒

実験手順

A mixture of 32 parts of 4-(4-fluorobenzoyl)-α-methyl-1-piperidineacetonitrile and 400 parts of methanol, saturated with ammonia is hydrogenated in the Parr-apparatus at 25° C. with 5 parts of Raney-nickel catalyst. After the calculated amount of hydrogen is taken up, the catalyst is filtered off and the filtrate is evaporated. The residue is taken up in methylbenzene and the latter is evaporated again. The residue is dissolved in 2,2'-oxybispropane and the solution is filtered till clear. The solvent is evaporated, yielding 32 parts (100%) of [1-(2-amino-1-methylethyl)-4-piperidinyl] (4-fluorophenyl)methanone as an oily residue.

後処理

  1. filtrationthe catalyst is filtered off
  2. customthe filtrate is evaporated
  3. customthe latter is evaporated again
  4. dissolutionThe residue is dissolved in 2,2'-oxybispropane
  5. filtrationthe solution is filtered till clear
  6. customThe solvent is evaporated

出典と根拠

ORDレコード
ord-82b236396d184543a936b2bc844e477c
出典データセット
uspto-grants-1982_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04335127

反応ノート

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