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Hydrochloric Acid → HCID 86754159, 화합물

HRID 580891
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HRID 580891 반응식
[CH3:1][C:2]([CH3:21])([CH2:14][N:15]1[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]1)[CH2:3][O:4][NH:5][C:6]([C:8]1[CH:9]=[N:10][CH:11]=[CH:12][CH:13]=1)=N.[ClH:22].N([O-])=O.[Na+].[OH-].[Na+]>O>[CH3:1][C:2]([CH3:21])([CH2:14][N:15]1[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]1)[CH2:3][O:4][N:5]=[C:6]([Cl:22])[C:8]1[CH:9]=[N:10][CH:11]=[CH:12][CH:13]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 23668193Sodium NitriteHCID 178454580HCID 178454580, 화합물

생성물 1

HCID 86754159HCID 86754159, 화합물

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

To a solution containing 2.23 g (7.63 mmoles) of N-(2,2-dimethyl-3-piperidinopropoxy)-3-pyridinecarboxamidine in 30 ml of a 1:1 mixture of concentrated hydrochloric acid and water, 2.63 g (38.2 mmoles) of sodium nitrite dissolved in 10 ml of water are dropwise added at 0° C. The reaction mixture is stirred at the same temperature for an additional 2 hours, then the pH value is adjusted to 12 by adding 2N sodium hydroxide solution, and the mixture is extracted twice with 30 ml of chloroform each. The organic phase is washed with 30 ml of water, dried over sodium sulfate, filtered and evaporated. The oily residue (1.83 g) is purified by column chromatography to give the title compound as a pale yellow oil in a yield of 1.62 g (68.5%).

후처리

  1. additionare dropwise added at 0° C
  2. extractionthe mixture is extracted twice with 30 ml of chloroform each
  3. washThe organic phase is washed with 30 ml of water
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. customevaporated
  7. customThe oily residue (1.83 g) is purified by column chromatography

출처 및 근거

ORD 기록
ord-b837eaa01339412488b61da201285736
출처 데이터셋
uspto-grants-1999_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05919796

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