Hydrazine hydrate (1:1) → 3-Methyl-2-phenylbutanehydrazide

HRID 388269ノート

反応式

HRID 388269 の反応式
[CH3:1][CH:2]([CH3:14])[CH:3]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:4](OC)=[O:5].O.[NH2:16][NH2:17]>>[CH3:1][CH:2]([CH3:14])[CH:3]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:4]([NH:16][NH2:17])=[O:5]

参加物

3

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 5051294Methyl 3-methyl-2-phenylbutanoate

生成物 1

HCID 591858993-Methyl-2-phenylbutanehydrazide収率 47%

実験手順

A stirred solution of methyl 3-methyl-2-phenylbutanoate (0.87 g, 1 eq) and hydrazine hydrate (10 mL) was heated at 110° C. for 12 h. The reaction mixture was then cooled and the solvents removed under reduced pressure. The crude oil was diluted with EtOAc and washed with H2O and the organic phase dried over Na2SO4, filtered, and the solvents removed under reduced pressure to yield a yellow oil (0.17 g, 47%) that was purified by column chromatography over silica gel to yield the product (0.61 g).

後処理

  1. temperatureThe reaction mixture was then cooled
  2. customthe solvents removed under reduced pressure
  3. additionThe crude oil was diluted with EtOAc
  4. washwashed with H2O
  5. dry with materialthe organic phase dried over Na2SO4
  6. filtrationfiltered
  7. customthe solvents removed under reduced pressure

出典と根拠

ORDレコード
ord-5f8a95886bd140b7b291494a4efa12d1
出典データセット
uspto-grants-2013_02
特許番号
US08377930B2

反応ノート

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