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Sodium Hydroxide → HCID 13825050、化合物

HRID 648505
ノート
印刷プレビュー

反応式

HRID 648505 の反応式
[Cl:1]C1C=CC=C(C(OO)=[O:9])C=1.Cl.Cl.[N:14]1[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=1[S:20][CH:21]1[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]1.[OH-].[Na+]>O>[ClH:1].[N:14]1[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=1[S:20]([CH:21]1[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]1)=[O:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 70297m-Chloroperbenzoic acid2 回HCID 135640052-(Piperidin-4-ylsulfanyl)pyridine dihydrochloride

生成物 1

HCID 13825050HCID 13825050、化合物収率 75.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

m-Chloroperbenzoic acid (0.77 g) was added to an ice-cooled solution of 4-[(2-pyridyl)thio]piperidine dihydrochloride (1.0 g) in water (20 ml) and the mixture was stirred at the same temperature for 7.5 hours. After additional m-chloroperbenzoic acid (0.07 g) and water (5 ml) were added, the mixture was stirred at the same temperature for 1 hour, adjusted to alkaline pH with sodium hydroxide solution, and extracted several times with chloroform. The extracts were combined, dried over magnesium sulfate, and concentrated in vacuo. The oily residue was dissolved in chloroform. The solution was treated with ethanolic hydrochloric acid and concentrated in vacuo. The crystalline residue was washed with isopropanol to give 4-[(2-pyridyl)sulfinyl]piperidine hydrochloride (0.70 g).

後処理

  1. stirringthe mixture was stirred at the same temperature for 1 hour
  2. extractionextracted several times with chloroform
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. dissolutionThe oily residue was dissolved in chloroform
  6. additionThe solution was treated with ethanolic hydrochloric acid
  7. concentrationconcentrated in vacuo
  8. washThe crystalline residue was washed with isopropanol

出典と根拠

ORDレコード
ord-55c1c39f86ce467c9e67ca66bdb40750
出典データセット
uspto-grants-1988_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04735952

反応ノート

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