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

HRID 2426964ノート

反応式

HRID 2426964 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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

後処理

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

出典と根拠

ORDレコード
ord-1cb772ebd4a04056a21e5f0a08731bfb
出典データセット
uspto-grants-2011_06
特許番号
US07968572B2

反応ノート

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