Sodium Hydroxide → HCID 13825045, 화합물

HRID 648514노트

반응식

HRID 648514 반응식
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

참가 물질

5

반응물 3

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

생성물 1

HCID 13825045HCID 13825045, 화합물수율 90.8%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-09af10bf57a74df392acd0c5cc89614d
출처 데이터셋
uspto-grants-1988_04
특허 번호
US04735952

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