Hydrochloric Acid → 2'-isopropyl-4',6'-dihydrospiro[piperidine-4,5'-pyrazolo[3,4-c]pyridin]-7'(2'H)-one hydrochloride

HRID 711033노트

반응식

HRID 711033 반응식
[CH:1]([N:4]1[CH:12]=[C:11]2[C:6]([C:7](=[O:25])[NH:8][C:9]3([CH2:17][CH2:16][N:15](C(OC(C)(C)C)=O)[CH2:14][CH2:13]3)[CH2:10]2)=[N:5]1)([CH3:3])[CH3:2].[ClH:26]>C(OCC)(=O)C.O1CCOCC1>[ClH:26].[CH:1]([N:4]1[CH:12]=[C:11]2[C:6]([C:7](=[O:25])[NH:8][C:9]3([CH2:13][CH2:14][NH:15][CH2:16][CH2:17]3)[CH2:10]2)=[N:5]1)([CH3:3])[CH3:2]

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 67491432Tert-butyl 2'-isopropyl-7'-oxo-2',4',6',7'-tetrahydrospiro[piperidine-4,5'-pyrazolo[3,4-c]pyridine]-1-carboxylate

생성물 1

HCID 674915642'-isopropyl-4',6'-dihydrospiro[piperidine-4,5'-pyrazolo[3,4-c]pyridin]-7'(2'H)-one hydrochloride

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매HCID 312751,4-Dioxane용매

실험 절차

To a solution of tert-butyl 2′-isopropyl-7′-oxo-2′,4′,6′,7′-tetrahydrospiro[piperidine-4,5′-pyrazolo[3,4-c]pyridine]-1-carboxylate (130 mg, 0.37 mmol) in ethyl acetate (5 mL) was added 4 M hydrochloric acid (2 mL) in 1,4-dioxane. The reaction mixture was stirred 3 hours at room temperature, the volatiles were removed under reduced pressure and the resultant residue was triturated with 10 mL heptane. The solid was dried under reduced pressure to yield 2′-isopropyl-4′,6′-dihydrospiro[piperidine-4,5′-pyrazolo[3,4-c]pyridin]-7′(2′H)-one hydrochloride (105 mg) as an off-white solid. +ESI (M+H) 249.1; 1H NMR (500 MHz, DMSO-d6, δ): 7.91 (s, 1H) 7.69 (s, 1H) 4.48-4.62 (m, 1H) 3.02-3.28 (m, 4H) 2.78 (s, 2H) 1.74-1.89 (m, 4H) 1.41 (d, J=6.59 Hz, 6H).

후처리

  1. customthe volatiles were removed under reduced pressure
  2. customthe resultant residue was triturated with 10 mL heptane
  3. customThe solid was dried under reduced pressure

출처 및 근거

ORD 기록
ord-be846f8eb3ad4c5f842afd2e738becca
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09181252B2

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