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Hydroxylamine → 7-nitro-3,4-dihydro-2H-naphthalen-1-one oxime

HRID 74089
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인쇄 미리보기

반응식

HRID 74089 반응식
[N+:1]([C:4]1[CH:13]=[C:12]2[C:7]([CH2:8][CH2:9][CH2:10][C:11]2=O)=[CH:6][CH:5]=1)([O-:3])=[O:2].[NH2:15][OH:16]>N1C=CC=CC=1>[N+:1]([C:4]1[CH:13]=[C:12]2[C:7]([CH2:8][CH2:9][CH2:10][C:11]2=[N:15][OH:16])=[CH:6][CH:5]=1)([O-:3])=[O:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 787HydroxylamineHCID 384457-Nitro-1-tetralone

생성물 1

HCID 3000317-nitro-3,4-dihydro-2H-naphthalen-1-one oxime수율 88%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

To a solution of 7-nitro-3,4-dihydro-2H-naphthalen-1-one (500 mg, 2.62 mmol) in pyridine (2 mL) was added hydroxylamine solution (1 mL, 50% solution in water). The reaction was stirred at room temperature for 1 h, then concentrated and purified by column chromatography (10-50% ethyl acetate-hexanes) to yield 7-nitro-3,4-dihydro-2H-naphthalen-1-one oxime (471 mg, 88%). HPLC ret. time 2.67 min, 10-99% CH3CN, 5 min run; ESI-MS 207.1 m/z (MH+).

후처리

  1. concentrationconcentrated
  2. custompurified by column chromatography (10-50% ethyl acetate-hexanes)

출처 및 근거

ORD 기록
ord-6ab0b14c88ce44db86f52083aa51a57e
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08829204B2

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