Methane → 4-Acetamidopiperidine dihydrochloride

HRID 266749

반응식

HRID 266749 반응식
[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]

참가 물질

7

반응물 4

HCID 297MethaneHCID 313Hydrochloric AcidHCID 12641850N-(1-Benzylpiperidin-4-yl)acetamideHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 114011054-Acetamidopiperidine dihydrochloride

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

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). δ 9.72(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)+.

후처리

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

출처 및 근거

ORD 기록
ord-014344128e7e4fcaa064e4e6ab988dc3
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05652242

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