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Hydrochloric Acid → 3-Chloro-5-(1-hydroxyethyl)-2-methylthiopyridine

HRID 2302236
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HRID 2302236 반응식
[C:1]([C:4]1[CH:5]=[C:6]([Cl:12])[C:7]([S:10][CH3:11])=[N:8][CH:9]=1)(=[O:3])[CH3:2].[BH4-].[Na+].Cl>C(O)C.O>[Cl:12][C:6]1[C:7]([S:10][CH3:11])=[N:8][CH:9]=[C:4]([CH:1]([OH:3])[CH3:2])[CH:5]=1
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참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 4311764Sodium borohydrideHCID 184358025-Acetyl-3-chloro-2-methylthiopyridine

생성물 1

HCID 184358003-Chloro-5-(1-hydroxyethyl)-2-methylthiopyridine수율 90%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

5-Acetyl-3-chloro-2-methylthiopyridine (24.1 g, 0.12 mol) was slurried in absolute ethanol (200 mL) and sodium borohydride (4.5 g, 0.118 mol) added in portions. The reaction mixture was stirred at room temperature for 48 hours and acidified to pH 2 with 2N hydrochloric acid. This was then diluted with water (200 mL) and the bulk of the ethanol evaporated under reduced pressure, the temperature of the mixture being maintained below 50° C. The reaction mixture was diluted with water (200 mL) and extracted twice with dichloromethane (15 mL). The combined organic extracts were washed with water (200 mL) and saturated sodium chloride solution (100 mL), dried over anhydrous sodium sulphate, and evaporated to dryness to give the desired product (21.9 g, 90%) as an orange oil.

후처리

  1. customthe bulk of the ethanol evaporated under reduced pressure
  2. temperaturethe temperature of the mixture being maintained below 50° C
  3. additionThe reaction mixture was diluted with water (200 mL)
  4. extractionextracted twice with dichloromethane (15 mL)
  5. washThe combined organic extracts were washed with water (200 mL) and saturated sodium chloride solution (100 mL)
  6. dry with materialdried over anhydrous sodium sulphate
  7. customevaporated to dryness

출처 및 근거

ORD 기록
ord-e002428224e44d6f8e7dfc0f1691a199
출처 데이터셋
uspto-grants-2002_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06432951B1

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