Hydroxyamine hydrochloride → N-hydroxy-1-[3-(methoxymethyl)phenyl]-1-(1-methyl-1H-tetrazol-5-yl)methanimine

HRID 452570노트

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HRID 452570 반응식
[CH3:1][O:2][CH2:3][C:4]1[CH:5]=[C:6]([C:10]([C:12]2[N:16]([CH3:17])[N:15]=[N:14][N:13]=2)=O)[CH:7]=[CH:8][CH:9]=1.Cl.[NH2:19][OH:20]>N1C=CC=CC=1>[OH:20][N:19]=[C:10]([C:6]1[CH:7]=[CH:8][CH:9]=[C:4]([CH2:3][O:2][CH3:1])[CH:5]=1)[C:12]1[N:16]([CH3:17])[N:15]=[N:14][N:13]=1

참가 물질

4

반응물 2

HCID 443297Hydroxyamine hydrochlorideHCID 67075295[3-(methoxymethyl)phenyl](1-methyl-1H-tetrazol-5-yl)methanone

생성물 1

HCID 136337384N-hydroxy-1-[3-(methoxymethyl)phenyl]-1-(1-methyl-1H-tetrazol-5-yl)methanimine수율 99.5%

시약·촉매·용매 1

HCID 1049Pyridine용매

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온도
70 °C

실험 절차

To a stirred solution of [3-(methoxymethyl)phenyl](1-methyl-1H-tetrazol-5-yl)methanone (7.17 g, 31 mmol) in dry pyridine (50 mL) was added hydroxylamine hydrochloride (5.36 g, 77 mmol). The reaction mixture was stirred at 70° C. for 4 h, then concentrated in vacuo and diluted with ethyl acetate (200 mL) and water (100 mL). The organic layer was separated, washed with water (100 mL) and dried (MgSO4). Evaporation of the solvent in vacuo afforded N-hydroxy-1-[3-(methoxymethyl)phenyl]-1-(1-methyl-1H-tetrazol-5-yl)methanimine as a yellow oil [8.43 g, yield 99.5%; HPLC/MS:m/z=248 (M+H); log P(HCOOH)=1.54].

후처리

  1. concentrationconcentrated in vacuo
  2. additiondiluted with ethyl acetate (200 mL) and water (100 mL)
  3. customThe organic layer was separated
  4. washwashed with water (100 mL)
  5. dry with materialdried (MgSO4)
  6. customEvaporation of the solvent in vacuo

출처 및 근거

ORD 기록
ord-07d4aa6ec66b4381acd39db0f638caf0
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08492388B2

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