Tin tetrachloride → HCID 82468131、化合物

HRID 1508862

反応式

HRID 1508862 の反応式
[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

参加物

5

反応物 2

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

生成物 1

HCID 82468131HCID 82468131、化合物収率 73.9%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 14798Sodium Hydroxide溶媒

反応条件

温度
50 °C

実験手順

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]+.

後処理

  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

出典と根拠

ORDレコード
ord-7ecaa61db4b94a3287c53b43cfc33c08
出典データセット
uspto-grants-2015_12
特許番号
US09221843B2

関連ノート

読み込み中…