Tin tetrachloride → HCID 82468131, 화합물

HRID 1508862

반응식

HRID 1508862 반응식
[N+:1]([C:4]1[CH:15]=[CH:14][C:7]([CH2:8][C:9]2[O:10][CH:11]=[CH:12][N:13]=2)=[CH:6][CH:5]=1)([O-])=O.[Sn](Cl)(Cl)(Cl)Cl>C(O)C.[OH-].[Na+]>[O:10]1[CH:11]=[CH:12][N:13]=[C:9]1[CH2:8][C:7]1[CH:14]=[CH:15][C:4]([NH2:1])=[CH:5][CH:6]=1

참가 물질

5

반응물 2

HCID 24287Tin tetrachlorideHCID 901105832-(4-Nitrobenzyl)oxazole

생성물 1

HCID 82468131HCID 82468131, 화합물수율 73.9%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 14798Sodium Hydroxide용매

반응 조건

온도
50 °C

실험 절차

To a solution of 2-(4-nitrobenzyl)oxazole (0.108 g, 0.59 mmol) in ethanol (3 mL) was added tin chloride (0.531 g, 2.35 mmol) and the mixture was stirred at 50° C. for 3 h. After this time, the reaction mixture was cooled, diluted with 1M sodium hydroxide, and extracted with ethyl acetate. The combined organic layer was dried over anhydrous sodium sulfate, filtered, and the filtrate was concentrated to afford the title compound (0.076 g, 63%) as a yellow oil. MW=174.20. 1H NMR (CD3OD, 500 MHz) δ 7.78 (d, J=0.8 Hz, 1H), 7.05 (d, J=0.8 Hz, 1H), 7.02-6.97 (m, 2H), 6.69-6.65 (m, 2H), 3.97 (s, 2H); APCI MS m/z 175 [M+H]+.

후처리

  1. temperatureAfter this time, the reaction mixture was cooled
  2. extractionextracted with ethyl acetate
  3. dry with materialThe combined organic layer was dried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. concentrationthe filtrate was concentrated

출처 및 근거

ORD 기록
ord-7ecaa61db4b94a3287c53b43cfc33c08
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09221843B2

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