Hydrazine hydrate (1:1) → tert-Butyl (aminooxy)acetate

HRID 414866ノート

反応式

HRID 414866 の反応式
[C:1]([O:5][C:6]([CH2:8][O:9][N:10]1C(=O)C2=CC=CC=C2C1=O)=[O:7])([CH3:4])([CH3:3])[CH3:2].O.NN>ClCCl>[C:1]([O:5][C:6]([CH2:8][O:9][NH2:10])=[O:7])([CH3:4])([CH3:3])[CH3:2]

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)2 回HCID 12919120Tert-butyl 2-(1,3-dioxoisoindolin-2-yloxy)acetate

生成物 1

HCID 12919121tert-Butyl (aminooxy)acetate収率 95.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

In 1.35 l of dichloromethane is dissolved 37.4 g (0.135 mole) of N-(tert-butoxycarbonylmethoxy) phthalimide, and 9.21 ml (0.189 mole) of hydrazine hydrate is added dropwise to the solution over the period of 10 minutes, followed by stirring at room temperature for 2 hours. 3.95 ml (0.081 mole) of hydrazine hydrate is furthermore added, followed by stirring for further 1.5 hours. The reaction solution is filtered, and the filtrate is washed with 300 ml of 2N ammonium water and aqueous sodium chloride solution successively, and dried over anhydrous sodium sulfate. The solvent is distilled off under reduced pressure to give 18.95 g (95.4%) of O-(tert-butoxycarbonylmethyl)hydroxylamine as a yellow oily product.

後処理

  1. additionis added dropwise to the solution over the period of 10 minutes
  2. stirringby stirring for further 1.5 hours
  3. filtrationThe reaction solution is filtered
  4. washthe filtrate is washed with 300 ml of 2N ammonium water and aqueous sodium chloride solution successively
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationThe solvent is distilled off under reduced pressure

出典と根拠

ORDレコード
ord-9aa65a6bfbf94f5d90510cbef3e8d95b
出典データセット
uspto-grants-1988_12
特許番号
US04794108

反応ノート

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