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Ammonia → HCID 15965878, 화합물

HRID 1665135
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HRID 1665135 반응식
[Cl-].[NH4+:2].[NH3:3].[CH2:4]([N:11]1[CH2:16][CH2:15][C:14](=O)[CH2:13][CH2:12]1)[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.[C-:18]#N.[Na+]>O>[NH2:2][CH2:18][C:14]1([NH2:3])[CH2:15][CH2:16][N:11]([CH2:4][C:5]2[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=2)[CH2:12][CH2:13]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 222AmmoniaHCID 8929Sodium CyanideHCID 192201-Benzyl-4-piperidoneHCID 25517Ammonium Chloride

생성물 1

HCID 15965878HCID 15965878, 화합물

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

To a solution of ammonium chloride (1.73 g, 32.3 mmol) in water (20 ml) is added a 30% ammonia solution (2 ml) followed by 1-benzyl-4-piperidone. After 20 minutes sodium cyanide (1.47 g, 30 mmol) is added portionwise over 15 minutes. After stirring for one hour, water (50 ml) is added and the products are extracted with DCM (3×50 ml), dried (MgSO4) filtered and concentrated in vacuo. Purification by chromatography on silica eluting with 50-100% EtOAc in iso-hexane affords 4-Aminomethyl-1-benzyl-piperidine-4-ylamine; [M+H]+ 216

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후처리

  1. extractionthe products are extracted with DCM (3×50 ml)
  2. dry with materialdried (MgSO4)
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customPurification by chromatography on silica eluting with 50-100% EtOAc in iso-hexane

출처 및 근거

ORD 기록
ord-69b56eaa12cc40e8ab8d2e4a7cbbb642
출처 데이터셋
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08039472B2

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