Sodium Sulfate → Methyl 4-(hydroxymethyl)oxane-4-carboxylate

HRID 2426964노트

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HRID 2426964 반응식
[O:1]1[CH2:6][CH2:5][C:4]([C:11](OC)=[O:12])([C:7]([O:9][CH3:10])=[O:8])[CH2:3][CH2:2]1.S([O-])([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[OH:12][CH2:11][C:4]1([C:7]([O:9][CH3:10])=[O:8])[CH2:5][CH2:6][O:1][CH2:2][CH2:3]1

참가 물질

4

반응물 2

HCID 24436Sodium SulfateHCID 11063483Dimethyl Tetrahydropyran-4,4-dicarboxylate

생성물 1

HCID 67253252Methyl 4-(hydroxymethyl)oxane-4-carboxylate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

Under an atmosphere of argon, to a solution of lithium aluminum tri(tert-butoxy)hydride (1.93 g) in tetrahydrofuran (15 mL) was added a solution of dimethyl tetrahydro-2H-pyran-4,4-dicarboxylate (606 mg) in tetrahydrofuran (5 mL) and the mixture was stirred at room temperature for an hour. To the reaction mixture was added an an aqueous saturated sodium sulfate solution till being cloudy. An insoluble matter was filtered and the filtrate was concentrated. The obtained residue was purified by column chromatography on silica gel (hexane:ethyl acetate=2:1→1:2→1:4→ethyl

후처리

  1. filtrationAn insoluble matter was filtered
  2. concentrationthe filtrate was concentrated
  3. customThe obtained residue was purified by column chromatography on silica gel (hexane

출처 및 근거

ORD 기록
ord-1cb772ebd4a04056a21e5f0a08731bfb
출처 데이터셋
uspto-grants-2011_06
특허 번호
US07968572B2

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