Hydrochloric Acid → Piperidine-4-carboxylic acid [6-(2-methoxy-phenyl)-pyrimidin-4-yl]-amide hydrochloride

HRID 1020050노트

반응식

HRID 1020050 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9]1[N:14]=[CH:13][N:12]=[C:11]([NH:15][C:16]([CH:18]2[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]2)=[O:17])[CH:10]=1.[ClH:24]>O1CCOCC1>[ClH:24].[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9]1[N:14]=[CH:13][N:12]=[C:11]([NH:15][C:16]([CH:18]2[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]2)=[O:17])[CH:10]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 59508946Piperidine-4-carboxylic acid [6-(2-methoxy-phenyl)-pyrimidin-4-yl]amide

생성물 1

HCID 67184524Piperidine-4-carboxylic acid [6-(2-methoxy-phenyl)-pyrimidin-4-yl]-amide hydrochloride

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

Piperidine-4-carboxylic acid [6-(2-methoxy-phenyl)-pyrimidin-4-yl]amide (compound #6A) (2.0 g, 6.4 mmol) was dissolved in a saturated solution of HCl in 1,4-dioxane (50 ml) and the clear solution was stirred at room temperature for half an hour. A pale yellow solid precipitated out. Diethyl ether (50 ml) was added to precipitate more of the solid. After filtration, the solid was washed with diethyl ether (50 ml) and dried under high vacuum to obtain piperidine-4-carboxylic acid [6-(2-methoxy-phenyl)-pyrimidin-4-yl]-amide hydrochloride (compound #14A, HCl salt of compound #6A), 2.2 g, 98%) as a white solid.

후처리

  1. customA pale yellow solid precipitated out
  2. additionDiethyl ether (50 ml) was added
  3. customto precipitate more of the solid
  4. filtrationAfter filtration
  5. washthe solid was washed with diethyl ether (50 ml)
  6. customdried under high vacuum

출처 및 근거

ORD 기록
ord-456c0ffd3ce74494b385458eda4ab5fc
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08716296B2

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