Hydrochloric Acid → 5,6-dihydro-2H-thiopyran-3-carboxylic acid

HRID 1053965노트

반응식

HRID 1053965 반응식
[S:1]1[CH2:6][CH2:5][CH:4]=[C:3]([C:7]([O:9]C)=[O:8])[CH2:2]1.CO.[OH-].[Li+].Cl>O.C1COCC1>[S:1]1[CH2:6][CH2:5][CH:4]=[C:3]([C:7]([OH:9])=[O:8])[CH2:2]1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 3939Lithium HydroxideHCID 10351950Methyl 5,6-dihydro-2H-thiopyran-3-carboxylate

생성물 1

HCID 102409305,6-dihydro-2H-thiopyran-3-carboxylic acid

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of methyl 5,6-dihydro-2H-thiopyran-3-carboxylate (1.0 g, 6.32 mmol) in 10:1 MeOH:THF (16.5 mL) was added lithium hydroxide (0.30 g, 13 mmol) in water (15 mL). The resulting mixture was stirred at ambient temperature for 4 hours. The reaction mixture was carefully acidified with 1N aqueous HCl, and extracted with EtOAc (3×). The combined organic extracts were washed with brine, dried over anhydrous Na2SO4, filtered, and concentrated in vacuo to afford the title compound. The residue was carried forward without further purification.

후처리

  1. extractionextracted with EtOAc (3×)
  2. washThe combined organic extracts were washed with brine
  3. dry with materialdried over anhydrous Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-923c220d7c074c7a8a8c7586d40c0824
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09394282B2

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