Hydroxylamine HCl → N-hydroxy-1-(1-methyl-1H-tetrazol-5-yl)-1-phenylmethanimine

HRID 350956

반응식

HRID 350956 반응식
[CH3:1][N:2]1[C:6]([C:7]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=O)=[N:5][N:4]=[N:3]1.[Cl-].[OH:16][NH3+:17]>N1C=CC=CC=1>[CH3:1][N:2]1[C:6]([C:7]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[N:17][OH:16])=[N:5][N:4]=[N:3]1

참가 물질

4

반응물 2

HCID 21645Hydroxylamine HClHCID 12331986(1-methyl-1H-tetrazol-5-yl)(phenyl)methanone

생성물 1

HCID 135990939N-hydroxy-1-(1-methyl-1H-tetrazol-5-yl)-1-phenylmethanimine수율 100%

시약·촉매·용매 1

HCID 1049Pyridine용매

반응 조건

온도
45 °C

실험 절차

(1-methyltetrazol-5-yl)phenylmethanone (11.1 g, 59.1 mmol) and hydroxylammonium chloride (10.3 g, 148 mmol) were added to 100 ml of pyridine, followed by stirring at 45° C. for 24 hours. After the completion of the reaction, the reaction solution was concentrated under reduced pressure and water and ethyl acetate were added to the resulting residue, and then the reaction product was extracted. The organic layer was washed in turn with dilute hydrochloric acid, water and an aqueous sodium hydrogencarbonate, and the organic layer was dried over anhydrous magnesium sulfate. The solvent was distilled off from the organic layer to obtain (1-methyltetrazol-5-yl)phenylmethanoneoxime (12.0 g, yield: 100%) represented by the formua:

후처리

  1. customAfter the completion of the reaction
  2. concentrationthe reaction solution was concentrated under reduced pressure and water and ethyl acetate
  3. additionwere added to the resulting residue
  4. extractionthe reaction product was extracted
  5. washThe organic layer was washed in turn with dilute hydrochloric acid, water
  6. dry with materialan aqueous sodium hydrogencarbonate, and the organic layer was dried over anhydrous magnesium sulfate
  7. distillationThe solvent was distilled off from the organic layer

출처 및 근거

ORD 기록
ord-ed8ca4e8b684411eb7408c665a9f1654
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07183299B2

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