Methane → 4-Acetamidopiperidine dihydrochloride

HRID 1290524

反応式

HRID 1290524 の反応式
[C:1]([NH:4][CH:5]1[CH2:10][CH2:9][N:8](CC2C=CC=CC=2)[CH2:7][CH2:6]1)(=[O:3])[CH3:2].[ClH:18].[H][H].C>[Pd].CO>[ClH:18].[C:1]([NH:4][CH:5]1[CH2:10][CH2:9][NH:8][CH2:7][CH2:6]1)(=[O:3])[CH3:2]

参加物

7

反応物 4

HCID 297MethaneHCID 313Hydrochloric AcidHCID 12641850N-(1-Benzylpiperidin-4-yl)acetamideHCID 178418361HCID 178418361、化合物

生成物 1

HCID 114011054-Acetamidopiperidine dihydrochloride

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

10% w/w Palladium on charcoal (1.5 g) was added to a solution of the product from step i) (10.0 g), 1 molar hydrochloric acid (21.5 ml) and methanol (150 ml) and the mixture hydrogenated at room temperature and pressure until the theoretical amount of hydrogen had been taken up. Charcoal was added, the mixture stirred for 1 hour then filtered through diatomaceous earth and the filtrate evaporated to dryness giving 4-acetylaminopiperidine hydrochloride, 8.64 g, as a sticky foam; NMR (CDCl3 +d6DMSO) δ9.72(1H,b), 9.02(1H,b), 7.40(1H,bd), 3.87(1H,m), 3.30(2H,m), 2.81(2H,m), 1.86(4H,m), 1.80(3H,s); m/e 143 (M+H)+.

後処理

  1. customhydrogenated at room temperature
  2. filtrationthen filtered through diatomaceous earth
  3. customthe filtrate evaporated to dryness

出典と根拠

ORDレコード
ord-021e71cb5cff47818031be31b9c5a77c
出典データセット
uspto-grants-1998_05
特許番号
US05750754

関連ノート

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