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

HRID 414866노트

반응식

HRID 414866 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 12919121tert-Butyl (aminooxy)acetate수율 95.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9aa65a6bfbf94f5d90510cbef3e8d95b
출처 데이터셋
uspto-grants-1988_12
특허 번호
US04794108

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