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HCID 10381067、化合物 → 4-Piperidinol, 1-(4-piperidinylacetyl)-

HRID 2184223
ノート
印刷プレビュー

反応式

HRID 2184223 の反応式
C([N:8]1[CH2:13][CH2:12][CH:11]([CH2:14][C:15]([N:17]2[CH2:22][CH2:21][CH:20]([OH:23])[CH2:19][CH2:18]2)=[O:16])[CH2:10][CH2:9]1)C1C=CC=CC=1.[H][H]>[C].[Pd].CC(O)C>[NH:8]1[CH2:9][CH2:10][CH:11]([CH2:14][C:15]([N:17]2[CH2:18][CH2:19][CH:20]([OH:23])[CH2:21][CH2:22]2)=[O:16])[CH2:12][CH2:13]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

5

反応物 2

HCID 10381067HCID 10381067、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 100366514-Piperidinol, 1-(4-piperidinylacetyl)-収率 89.4%

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 3776Isopropanol溶媒

反応条件

温度
80 °C

実験手順

14.2 g (0.05 mol) of 1-(1-benzyl-4-piperidylacetyl)-4-hydroxypiperidine [1] and 127.9 g of 2-propanol were mixed with each other. To this mixture, 1.42 g of 5% palladium-carbon (containing water at 50% content) was added. The reaction was allowed to proceed for 14 hours at 50° C. under the flow of hydrogen. The catalyst was removed by filtration therefrom, and the filtrate was concentrated under a reduced pressure. 23.6 g of acetonitrile was added to the concentrated residue, and the temperature of the mixture was increased to a reflux temperature of 80° C. The crystals which precipitated at room temperature were collected by filtration and the resultant wet crystals were dried under a reduced pressure, whereby 9.08 g of the title compound in the state of white powder was obtained (the yield was 89.4%).

後処理

  1. customThe catalyst was removed by filtration
  2. concentrationthe filtrate was concentrated under a reduced pressure
  3. addition23.6 g of acetonitrile was added to the concentrated residue
  4. customThe crystals which precipitated at room temperature
  5. filtrationwere collected by filtration
  6. dry with materialthe resultant wet crystals were dried under a reduced pressure, whereby 9.08 g of the title compound in the state of white powder
  7. customwas obtained (the yield was 89.4%)

出典と根拠

ORDレコード
ord-3b2c0661508f4736bdadce193a56d520
出典データセット
uspto-grants-2005_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06900326B2

反応ノート

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