Hydrochloric Acid → 4-[(4-amino-2-ethyl-1H-imidazo[4,5-c][1,5]naphthyridin-1-yl)methyl]piperidin-4-ol dihydrochloride

HRID 44774

반응식

HRID 44774 반응식
[NH2:1][C:2]1[C:11]2[N:12]=[C:13]([CH2:30][CH3:31])[N:14]([CH2:15][C:16]3([OH:29])[CH2:21][CH2:20][N:19](C(OC(C)(C)C)=O)[CH2:18][CH2:17]3)[C:10]=2[C:9]2[N:8]=[CH:7][CH:6]=[CH:5][C:4]=2[N:3]=1.[ClH:32]>C(O)C>[ClH:32].[ClH:32].[NH2:1][C:2]1[C:11]2[N:12]=[C:13]([CH2:30][CH3:31])[N:14]([CH2:15][C:16]3([OH:29])[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]3)[C:10]=2[C:9]2[N:8]=[CH:7][CH:6]=[CH:5][C:4]=2[N:3]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 57515526tert-butyl 4-[(4-amino-2-ethyl-1H-imidazo[4,5-c][1,5]naphthyridin-1-yl)methyl]-4-hydroxypiperidine-1-carboxylate

생성물 1

HCID 575155314-[(4-amino-2-ethyl-1H-imidazo[4,5-c][1,5]naphthyridin-1-yl)methyl]piperidin-4-ol dihydrochloride

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
50 °C

실험 절차

Under a nitrogen atmosphere a mixture of tert-butyl 4-[(4-amino-2-ethyl-1H-imidazo[4,5-c][1,5]naphthyridin-1-yl)methyl]-4-hydroxypiperidine-1-carboxylate (6.00 g), aqueous hydrochloric acid (14 mL of 6M), and ethanol (56 mL) was heated at 50° C. overnight. The reaction mixture was concentrated under reduced pressure. The residue was concentrated from methanol 3 times, triturated with acetonitrile, isolated by filtration, washed with acetonitrile, and then dried under high vacuum to provide 5.55 g of 4-[(4-amino-2-ethyl-1H-imidazo[4,5-c][1,5]naphthyridin-1-yl)methyl]piperidin-4-ol dihydrochloride as a tan powder.

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. concentrationThe residue was concentrated from methanol 3 times
  3. customtriturated with acetonitrile
  4. customisolated by filtration
  5. washwashed with acetonitrile
  6. customdried under high vacuum

출처 및 근거

ORD 기록
ord-215ce135b4c546299bb936a820830a81
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08541438B2

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