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Hydrochloric Acid → 5-pyrrolidin-1-yl-7-(tetrahydro-2H-pyran-4-ylamino)pyrazolo[1,5-a]pyrimidine-2-carboxylic acid

HRID 869715
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인쇄 미리보기

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HRID 869715 반응식
[N:1]1([C:6]2[CH:11]=[C:10]([NH:12][CH:13]3[CH2:18][CH2:17][O:16][CH2:15][CH2:14]3)[N:9]3[N:19]=[C:20]([C:22]([O:24]CC)=[O:23])[CH:21]=[C:8]3[N:7]=2)[CH2:5][CH2:4][CH2:3][CH2:2]1.[OH-].[Na+].Cl>C(O)C.O1CCCC1>[N:1]1([C:6]2[CH:11]=[C:10]([NH:12][CH:13]3[CH2:14][CH2:15][O:16][CH2:17][CH2:18]3)[N:9]3[N:19]=[C:20]([C:22]([OH:24])=[O:23])[CH:21]=[C:8]3[N:7]=2)[CH2:5][CH2:4][CH2:3][CH2:2]1
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참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 67408425ethyl 5-pyrrolidin-1-yl-7-(tetrahydro-2H-pyran-4-ylamino)pyrazolo[1,5-a]pyrimidine-2-carboxylate

생성물 1

HCID 674075435-pyrrolidin-1-yl-7-(tetrahydro-2H-pyran-4-ylamino)pyrazolo[1,5-a]pyrimidine-2-carboxylic acid

시약·촉매·용매 2

HCID 702Ethanol용매
HCID 8028
Tetrahydrofuran
용매

실험 절차

To a solution of ethyl 5-pyrrolidin-1-yl-7-(tetrahydro-2H-pyran-4-ylamino)pyrazolo[1,5-a]pyrimidine-2-carboxylate (1.89 g, 5.26 mmol) in ethanol (25 mL) and tetrahydrofuran (25 mL) was added 1N aqueous sodium hydroxide (10.5 mL, 10.5 mmol) at room temperature. After being stirred for 23 h at same temperature, 6N aqueous hydrochloric acid (1.75 mL, 3.50 mmol), and then the reaction mixture was concentrated in vacuo. The residue was triturated with diisopropyl ether to give 5-pyrrolidin-1-yl-7-(tetrahydro-2H-pyran-4-ylamino)pyrazolo[1,5-a]pyrimidine-2-carboxylic acid. MS (APCI): m/z 330 (M−H).

후처리

  1. concentrationthe reaction mixture was concentrated in vacuo
  2. customThe residue was triturated with diisopropyl ether

출처 및 근거

ORD 기록
ord-457c0f508ec24934902457d327a44883
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08969376B2

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