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Hydrochloric Acid → 3-(Benzyloxy)-N-(4-methylthiazol-2-yl)-5-(1-phenylvinyl)pyridin-2-amine hydrochloride

HRID 1426159
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HRID 1426159 반응식
[CH2:1]([O:8][C:9]1[C:10]([NH:16][C:17]2[S:18][CH:19]=[C:20]([CH3:22])[N:21]=2)=[N:11][CH:12]=[C:13](Br)[CH:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Li]C.C([Li])CCC.[C:30]([C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1)(=O)[CH3:31].[ClH:39].C(=O)(O)[O-].[Na+]>>[ClH:39].[CH2:1]([O:8][C:9]1[C:10]([NH:16][C:17]2[S:18][CH:19]=[C:20]([CH3:22])[N:21]=2)=[N:11][CH:12]=[C:13]([C:30]([C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)=[CH2:31])[CH:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 6

HCID 313Hydrochloric Acid2회HCID 7410AcetophenoneHCID 516892Sodium BicarbonateHCID 16061466HCID 16061466, 화합물HCID 178418339ButyllithiumHCID 178418348HCID 178418348, 화합물

생성물 1

HCID 86639697
3-(Benzyloxy)-N-(4-methylthiazol-2-yl)-5-(1-phenylvinyl)pyridin-2-amine hydrochloride
수율 47.1%

실험 절차

3-(Benzyloxy)-5-bromo-N-(4-methylthiazol-2-yl)pyridin-2-amine (0.250 g, 0.664 mmol), MeLi (0.519 ml, 0.831 mmol), butyllithium (0.332 ml, 0.831 mmol), and acetophenone (0.0798 g, 0.664 mmol) were reacted according to the method of Example 7. 1M HCl was added and the reaction mixture was stirred at ambient temperature for 2 hours. The reaction mixture was poured onto ice and saturated sodium bicarbonate and extracted twice with dichloromethane. The organic layer was dried, filtered, and concentrated. The residue was purified by silica gel chromatography (5-10% EtOAc in hexane) to provide the title compound (0.125 g, 47.1% yield) after HCl salt formation. 1H NMR (DMSO-d6) δ 7.81 (d, 1H), 7.54 (m, 2H), 7.48 (m, 1H), 7.37 (m, 6H), 7.30 (m, 2H), 6.81 (s, 1H), 5.60 (s, 1H), 5.54 (s, 1H), 5.33 (s, 2H), 2.31 (s, 3H). Mass spectrum (apci) m/z=400.1 (M+H-HCl)

후처리

  1. extractionextracted twice with dichloromethane
  2. customThe organic layer was dried
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe residue was purified by silica gel chromatography (5-10% EtOAc in hexane)

출처 및 근거

ORD 기록
ord-56e224aa634d4db1a538ea8b99dd439b
출처 데이터셋
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08933077B2

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