Sodium Hydroxide → HCID 13825045、化合物

HRID 648514ノート

反応式

HRID 648514 の反応式
ClC1C=CC=C(C(OO)=[O:9])C=1.Cl.Cl.[N:14]1[CH:19]=[CH:18][C:17]([S:20][CH:21]2[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]2)=[CH:16][CH:15]=1.[OH-].[Na+]>O>[N:14]1[CH:19]=[CH:18][C:17]([S:20]([CH:21]2[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]2)=[O:9])=[CH:16][CH:15]=1

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 70297m-Chloroperbenzoic acidHCID 219060714-[(Piperidin-4-yl)sulfanyl]pyridine--hydrogen chloride (1/2)

生成物 1

HCID 13825045HCID 13825045、化合物収率 90.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

m-Chloroperbenzoic acid (1.20 g) was added to a stirred solution of 4-[(4-pyridyl)thio]piperidine dihydrochloride (1.33 g) in water (30 ml) under ice-cooling, and the mixture was stirred at the same temperature for 3 hours and then at room temperature for 5.5 hours. The resultant mixture was diluted with water and the pH of the mixture was adjusted to about 11 with 5% sodium hydroxide solution. The solution was extracted several times with chloroform. The extracts were combined, dried over magnesium sulfate, and concentrated in vacuo. The oily residue was crystallized from n-hexane and the crystals were recrystallized from a mixture of n-hexane and isopropanol to give 4-[(4-pyridyl)sulfinyl]piperidine (0.95 g).

後処理

  1. temperaturecooling
  2. waitat room temperature for 5.5 hours
  3. extractionThe solution was extracted several times with chloroform
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe oily residue was crystallized from n-hexane
  7. customthe crystals were recrystallized from a mixture of n-hexane and isopropanol

出典と根拠

ORDレコード
ord-09af10bf57a74df392acd0c5cc89614d
出典データセット
uspto-grants-1988_04
特許番号
US04735952

反応ノート

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