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Hydrochloric Acid → N-(4-(3-(piperidin-4-yl)pyrazin-2-yloxy)phenyl)pyridin-2-amine dihydrochloride

HRID 473709
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HRID 473709 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[NH:7][C:8]1[CH:33]=[CH:32][C:11]([O:12][C:13]2[C:14]([C:19]3[CH2:24][CH2:23][N:22](C(OC(C)(C)C)=O)[CH2:21][CH:20]=3)=[N:15][CH:16]=[CH:17][N:18]=2)=[CH:10][CH:9]=1.C(Cl)[Cl:35].[ClH:37]>O1CCOCC1>[ClH:35].[ClH:37].[NH:22]1[CH2:21][CH2:20][CH:19]([C:14]2[C:13]([O:12][C:11]3[CH:32]=[CH:33][C:8]([NH:7][C:2]4[CH:3]=[CH:4][CH:5]=[CH:6][N:1]=4)=[CH:9][CH:10]=3)=[N:18][CH:17]=[CH:16][N:15]=2)[CH2:24][CH2:23]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric Acid2회HCID 6344DichloromethaneHCID 59374036tert-butyl 4-(3-(4-(pyridin-2-ylamino)phenoxy)pyrazin-2-yl)-5,6-dihydropyridine-1(2H)-carboxylate

생성물 1

HCID 67425394N-(4-(3-(piperidin-4-yl)pyrazin-2-yloxy)phenyl)pyridin-2-amine dihydrochloride

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

To a solution of tert-butyl 4-(3-(4-(pyridin-2-ylamino)phenoxy)pyrazin-2-yl)-5,6-dihydropyridine-1(2H)-carboxylate (5.2 g, 11.67 mmol) and DCM (100 mL) was added 4M HCl in dioxane (12 mL, 48.0 mmol). After 4 hours, another 5 mL of 4M HCl in dioxane was added. After a further 16 hours, the precipitates had clung to the walls of the flask and the clear stirring solution was decanted away. The precipitates were washed with another 50 mL of DCM and the solution again decanted away. The flask was placed under vacuum for 30 minutes to give N-(4-(3-(piperidin-4-yl)pyrazin-2-yloxy)phenyl)pyridin-2-amine dihydrochloride as a hydroscopic yellow solid.

후처리

  1. waitAfter a further 16 hours
  2. customthe clear stirring solution was decanted away
  3. washThe precipitates were washed with another 50 mL of DCM
  4. customthe solution again decanted away
  5. waitThe flask was placed under vacuum for 30 minutes

출처 및 근거

ORD 기록
ord-e10ea50882b549f3973317976f9f5d2f
출처 데이터셋
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08637500B2

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