Water → 2-[(2,5-Dimethylphenyl)methylsulfonyl]pyridine

HRID 2300996ノート

反応式

HRID 2300996 の反応式
[CH3:1][C:2]1[CH:15]=[CH:14][C:13]([CH3:16])=[CH:12][C:3]=1[CH2:4][S:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][N:7]=1.ClC1C=CC=C(C(OO)=[O:25])C=1.[OH2:28]>C(Cl)(Cl)Cl>[CH3:1][C:2]1[CH:15]=[CH:14][C:13]([CH3:16])=[CH:12][C:3]=1[CH2:4][S:5]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][N:7]=1)(=[O:25])=[O:28]

参加物

5

反応物 3

HCID 962WaterHCID 70297m-Chloroperbenzoic acidHCID 5073012-[(2,5-Dimethylphenyl)methylsulfanyl]pyridine

生成物 1

HCID 5012402-[(2,5-Dimethylphenyl)methylsulfonyl]pyridine

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

To a well-stirred and cooled (−10° C.) solution of 6.9 g (0.03 mole) of 2-(2,5-dimethyl-benzylthio)pyridine in 75 ml of chloroform was added portion-wise a solution of 12 g (0.06 mole) of metachloroperbenzoic acid dissolved in 100 ml of chloroform. The mixture was kept at −10° C. for 10 minutes and then allowed to warm to room temperature over the next six hours. It was stirred at room temperature overnight. Water was then added and the phases separated. he chloroform phase was washed with aqueous sodium bicarbonate and then again with water. he chloroform phase was dried with anhydrous sodium sulfate, filtered, and the chloroform removed using a rotary evaporator to give 8 g of an oil. The oil was crystallized from a small amount of ethanol, with a melting point of 77-78° C., and a yield of 3 g (30%). IR spectrum showed the presence of SO2 at 1160, 1310 cm−1.

後処理

  1. stirringIt was stirred at room temperature overnight
  2. customthe phases separated
  3. washhe chloroform phase was washed with aqueous sodium bicarbonate
  4. dry with materialhe chloroform phase was dried with anhydrous sodium sulfate
  5. filtrationfiltered
  6. customthe chloroform removed
  7. customa rotary evaporator

出典と根拠

ORDレコード
ord-68f1ae8e5be1470bb31639fdb16b0fa7
出典データセット
uspto-grants-2002_12
特許番号
US06498254B1

反応ノート

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