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Hydrazine → Oxane-4-carbohydrazide

HRID 710943
ノート
印刷プレビュー

反応式

HRID 710943 の反応式
[O:1]1[CH2:6][CH2:5][CH:4]([C:7]([O:9]C)=O)[CH2:3][CH2:2]1.[NH2:11][NH2:12]>CO>[O:1]1[CH2:6][CH2:5][CH:4]([C:7]([NH:11][NH2:12])=[O:9])[CH2:3][CH2:2]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 9321HydrazineHCID 27735202H-Pyran-4-carboxylic acid, tetrahydro-, methyl ester

生成物 1

HCID 28064717Oxane-4-carbohydrazide収率 66.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of methyl tetrahydro-2H-pyran-4-carboxylate (1.44 g, 10.0 mmol) in methanol (50 mL) was stirred at 50° C. To the reaction mixture, hydrazine.monohydrate (0.675 g) was added, followed by stirring at the same temperature for 2 hours, after completion of the reaction, the reaction mixture was concentrated and diluted with methylene chloride, the solution was then washed with saturated sodium bicarbonate aqueous solution and saturated brine, and the organic layer was dried over magnesium sulfate and the solvent was distilled off under reduced pressure to afford 952 mg of the title compound (yield 66.1%).

後処理

  1. customafter completion of the reaction
  2. concentrationthe reaction mixture was concentrated
  3. additiondiluted with methylene chloride
  4. washthe solution was then washed with saturated sodium bicarbonate aqueous solution and saturated brine
  5. dry with materialthe organic layer was dried over magnesium sulfate
  6. distillationthe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-07c71cfcc2b64bec8a6a927da5a832e3
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09181250B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート