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Sodium Hydroxide → HCID 13825047、化合物

HRID 648500
ノート
印刷プレビュー

反応式

HRID 648500 の反応式
[Cl:1]C1C=CC=C(C(OO)=[O:9])C=1.Cl.[F:13][C: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.S(=O)(O)[O-].[Na+].[OH-].[Na+]>C(Cl)(Cl)Cl>[ClH:1].[F:13][C:14]1[CH:15]=[CH:16][C:17]([S:20]([CH:21]2[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]2)=[O:9])=[CH:18][CH:19]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 14798Sodium HydroxideHCID 70297m-Chloroperbenzoic acidHCID 136080004-[(4-Fluorophenyl)sulfanyl]piperidine--hydrogen chloride (1/1)HCID 23665763Sodium Bisulfite

生成物 1

HCID 13825047HCID 13825047、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

3-Chloroperbenzoic acid (0.96 g) was slowly added to a stirred solution of 4-[(4-fluorophenyl)thio]piperidine hydrochloride (I.2g) in chloroform (60 ml) under ice-cooling over a period of 5 minutes and the mixture was stirred at the same temperature for 45 minutes. After being treated with sodium bisulfite solution under ice-cooling, the resultant mixture was adjusted to alkaline pH with 20% sodium hydroxide solution. The chloroform layer was separated and the aqueous layer was extracted three times with chloroform. The chloroform layers were combined and dried over magnesium sulfate. After removal of magnesium sulfate, the solution was treated with ethereal hydrochloric acid and concentrated to dryness in vacuo. The powdery residue was washed with isopropanol to give 4-[(4-fluorophenyl)sulfinyl]piperidine hydrochloride (1.10 g) as colourless powser.

後処理

  1. temperaturecooling over a period of 5 minutes
  2. temperaturecooling
  3. customThe chloroform layer was separated
  4. extractionthe aqueous layer was extracted three times with chloroform
  5. dry with materialdried over magnesium sulfate
  6. customAfter removal of magnesium sulfate
  7. additionthe solution was treated with ethereal hydrochloric acid
  8. concentrationconcentrated to dryness in vacuo
  9. washThe powdery residue was washed with isopropanol

出典と根拠

ORDレコード
ord-a6c46c69459a4215934713eabf10bc2b
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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