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Hydrochloric Acid → HCID 58386254, 화합물

HRID 1893795
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HRID 1893795 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[C@H:9]1[CH2:13][CH2:12][CH2:11][N:10]1[C:14]1[CH:19]=[CH:18][N:17]2[N:20]=[CH:21][C:22]([NH:23][C:24]([C:26]3([C:29]([O:31]C)=[O:30])[CH2:28][CH2:27]3)=[O:25])=[C:16]2[N:15]=1.O.[OH-].[Li+].Cl>C1COCC1.CO.O.O>[F:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[C@H:9]1[CH2:13][CH2:12][CH2:11][N:10]1[C:14]1[CH:19]=[CH:18][N:17]2[N:20]=[CH:21][C:22]([NH:23][C:24]([C:26]3([C:29]([OH:31])=[O:30])[CH2:27][CH2:28]3)=[O:25])=[C:16]2[N:15]=1
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참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 168937Lithium hydroxide, monohydrateHCID 58386296(R)-methyl 1-(5-(2-(2,5-difluorophenyl)pyrrolidin-1-yl)pyrazolo[1,5-a]pyrimidin-3-ylcarbamoyl)cyclopropanecarboxylate

생성물 1

HCID 58386254HCID 58386254, 화합물수율 82.3%

시약·촉매·용매 2

HCID 962Water용매
HCID 21892291
Methanol tetrahydrofuran water
용매

실험 절차

(R)-methyl 1-(5-(2-(2,5-difluorophenyl)pyrrolidin-1-yl)pyrazolo[1,5-a]pyrimidin-3-ylcarbamoyl)cyclopropanecarboxylate (Example 33; 24 mg, 0.054 mmol), was dissolved in a mixture solvent of THF/MeOH/water (0.3/0.3/0.2 mL), followed by addition of lithium hydroxide monohydrate (6 mg, 0.14 mmol). After stirring at ambient temperature for five hours, the reaction mixture was diluted with water (15 mL), acidified with 1N HCl (aq.) to pH ˜3, and filtered, giving the final product as a fine white solid (19 mg, 82% yield). MS (apci) m/z=428.2 (M+H).

후처리

  1. filtrationfiltered

출처 및 근거

ORD 기록
ord-db07abe2547e4424b543861bc4506e19
출처 데이터셋
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08513263B2

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