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Sodium Bicarbonate → 4-(2-cyanopropan-2-yl)-N-(2-methyl-7-phenylpyrazolo[1,5-a]pyrimidin-5-yl)benzamide

HRID 1409255
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HRID 1409255 반응식
[CH3:1][C:2]1[CH:17]=[C:5]2[N:6]=[C:7]([NH2:16])[CH:8]=[C:9]([C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=3)[N:4]2[N:3]=1.[C:18]([C:20]([C:23]1[CH:31]=[CH:30][C:26]([C:27](Cl)=[O:28])=[CH:25][CH:24]=1)([CH3:22])[CH3:21])#[N:19].C([O-])(O)=O.[Na+]>N1C=CC=CC=1>[C:18]([C:20]([C:23]1[CH:24]=[CH:25][C:26]([C:27]([NH:16][C:7]2[CH:8]=[C:9]([C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=3)[N:4]3[N:3]=[C:2]([CH3:1])[CH:17]=[C:5]3[N:6]=2)=[O:28])=[CH:30][CH:31]=1)([CH3:22])[CH3:21])#[N:19]
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5

반응물 3

HCID 516892Sodium BicarbonateHCID 450819154-(2-Cyanopropan-2-yl)benzoyl chlorideHCID 582071812-Methyl-7-phenylpyrazolo[1,5-a]pyrimidin-5-amine

생성물 1

HCID 668789494-(2-cyanopropan-2-yl)-N-(2-methyl-7-phenylpyrazolo[1,5-a]pyrimidin-5-yl)benzamide수율 48%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

In a 50 ml pear flask was added 2-methyl-7-phenylpyrazolo[1,5-a]pyrimidin-5-amine (10A, 450 mg, 2.0 mmol) in pyridine (10 ml). To this mixture was added 4-(2-cyanopropan-2-yl)benzoyl chloride (550 mg, 2.6 mmol) and the mixture was stirred at room temperature for 2 h. Saturated NaHCO3 was then added and pyridine was removed in vacuo. The residue was partitioned between saturated NaHCO3 and ethyl acetate, and the aqueous layer was extracted one more time with ethyl acetate. Combined organic layers were dried over MgSO4, filtered and concentrated. The crude product was purified by column chromatography (SiO2, 15-25% EtOAc/hexanes) to give the titled compound (380 mg, 48%). 1H NMR (DMSO-d6) δ: 11.35 (s, 1H), 8.10-8.16 (m, 2H), 8.04-8.09 (m, 2H), 7.96 (s, 1H), 7.67-7.73 (m, 2H), 7.60-7.66 (m, 3H), 6.41 (s, 1H), 2.41 (s, 3H), 1.74 (s, 6H); ESI-MS: m/z 396.3 (M+H)+.

후처리

  1. custompyridine was removed in vacuo
  2. customThe residue was partitioned between saturated NaHCO3 and ethyl acetate
  3. extractionthe aqueous layer was extracted one more time with ethyl acetate
  4. dry with materialCombined organic layers were dried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe crude product was purified by column chromatography (SiO2, 15-25% EtOAc/hexanes)

출처 및 근거

ORD 기록
ord-76f9874631234bdbbae303437bf8f271
출처 데이터셋
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08921358B2

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