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Acetic Acid → HCID 10118434, 화합물

HRID 861119
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HRID 861119 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:21]([C:22]3[CH:27]=[CH:26][N:25]=[C:24]([NH:28][CH2:29][CH2:30][CH2:31][CH3:32])[N:23]=3)=[C:11]3[CH:12]=[CH:13][CH:14]=[C:15]([NH:16][CH2:17][CH2:18][CH2:19][CH3:20])[N:10]3[N:9]=2)=[CH:4][CH:3]=1.[C:33]1(=O)[CH2:38][CH2:37][CH2:36][CH2:35][CH2:34]1.C(O)(=O)C.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(=O)(O)[O-].[Na+]>ClCCCl.CCOCC>[CH2:17]([NH:16][C:15]1[N:10]2[N:9]=[C:8]([C:5]3[CH:4]=[CH:3][C:2]([NH:1][CH:33]4[CH2:38][CH2:37][CH2:36][CH2:35][CH2:34]4)=[CH:7][CH:6]=3)[C:21]([C:22]3[CH:27]=[CH:26][N:25]=[C:24]([NH:28][CH2:29][CH2:30][CH2:31][CH3:32])[N:23]=3)=[C:11]2[CH:12]=[CH:13][CH:14]=1)[CH2:18][CH2:19][CH3:20]
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참가 물질

8

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HCID 176Acetic AcidHCID 7967CyclohexanoneHCID 516892Sodium BicarbonateHCID 5049666Sodium triacetoxyborohydrideHCID 10113479N-{4-[2-(4-aminophenyl)-7-(butylamino)pyrazolo[1,5-a]pyridin-3-yl]-2-pyrimidinyl}-N-butylamine

생성물 1

HCID 10118434HCID 10118434, 화합물
수율 73%

시약·촉매·용매 2

HCID 111,2-Dichloroethane용매HCID 3283Diethyl Ether용매

실험 절차

A solution of N-{4-[2-(4-aminophenyl)-7-(butylamino)pyrazolo[1,5-a]pyridin-3-yl]-2-pyrimidinyl}-N-butylamine (62 mg, 0.15 mmol) in 1,2-dichloroethane (2 mL) was treated with cyclohexanone (0.02 mL, 0.22 mmol), acetic acid (0.04 mL, 0.72 mmol), and sodium triacetoxyborohydride (61 mg, 0.29 mmol). The resultant solution was stirred at room temperature for 18 hours. Saturated aqueous sodium bicarbonate was added dropwise followed by ether. The organic layer was washed with brine. The aqueous layer was extracted with ether and the combined organics dried over magnesium sulfate. Filtration and concentration followed by flash chromatography (4:1 to 2:1 hexanes-ethyl acetate) provided N-butyl-3-[2-(butylamino)-4-pyrimidinyl]-2-[4-(cyclohexylamino)phenyl]pyrazolo[1,5-a]pyridin-7-amine (54 mg, 73%) as an orange oil. 1H NMR (CDCl3): δ 7.94 (d, 1 H), 7.73 (d, 1 H), 7.39 (d, 2 H), 7.23 (m, 1 H), 6.59 (d, 2 H), 6.41 (d, 1 H), 6.03 (m, 1 H), 5.91 (d, 1 H), 5.11 (broad, 1 H), 3.66 (broad, 1 H), 3.44 (m, 2 H), 3.30 (m, 3 H), 2.05 (m, 2 H), 1.75–1.12 (m, 16 H), 0.95–0.92 (m, 6 H); MS m/z 512 (M+1). This material was treated with anhydrous hydrochloric acid in ether to provide the corresponding hydrochloride salt.

후처리

  1. washThe organic layer was washed with brine
  2. extractionThe aqueous layer was extracted with ether
  3. dry with materialthe combined organics dried over magnesium sulfate
  4. filtrationFiltration and concentration

출처 및 근거

ORD 기록
ord-e03304976db242a7836b0d8841e70fac
출처 데이터셋
uspto-grants-2006_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07153855B2

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