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

HRID 537107ノート

反応式

HRID 537107 の反応式
[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]

参加物

5

反応物 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

生成物 1

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

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 312751,4-Dioxane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-98f7206943f44dc29b726f8179ddef75
出典データセット
uspto-grants-2014_10
特許番号
US08859773B2

反応ノート

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