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Sodium Hydroxide → HCID 13825050, 화합물

HRID 648505
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HRID 648505 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 70297m-Chloroperbenzoic acid2회HCID 135640052-(Piperidin-4-ylsulfanyl)pyridine dihydrochloride

생성물 1

HCID 13825050HCID 13825050, 화합물수율 75.8%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-55c1c39f86ce467c9e67ca66bdb40750
출처 데이터셋
uspto-grants-1988_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04735952

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