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Hydroxyamine hydrochloride → HCID 73654202, 화합물

HRID 2081206
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HRID 2081206 반응식
[F:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]2[C:14]=1[N:13]([CH3:15])[C:12]1[CH2:11][CH2:10][CH2:9][C:8](=O)[C:7]2=1.Cl.[NH2:18][OH:19]>N1C=CC=CC=1>[F:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]2[C:14]=1[N:13]([CH3:15])[C:12]1[CH2:11][CH2:10][CH2:9][C:8](=[N:18][OH:19])[C:7]2=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 443297Hydroxyamine hydrochlorideHCID 197698468-Fluoro-9-methyl-1,2,3,9-tetrahydro-4H-carbazol-4-one

생성물 1

HCID 73654202HCID 73654202, 화합물수율 56.1%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

A mixture of 8-fluoro-1,2,3,9-tetrahydro-9-methyl-4H-carbazol-4-one (3.0 g) and hydroxylamine hydrochloride (2.92 g) in pyridine (ca. 35 ml) was heated at 60° for 3 h. The solution was concentrated in vacuo then azeotropically dried with toluene (2×10 ml). The residue was treated with 8% sodium bicarbonate solution (125 ml) and extracted with ethyl acetate (3×100 ml). The combined extracts were filtered and concentrated in vacuo to give the title compound (1.8 g) as a solid, t.l.c. (System A, 100:8:1) Rf 0.66.

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후처리

  1. temperaturewas heated at 60° for 3 h
  2. concentrationThe solution was concentrated in vacuo
  3. dry with materialthen azeotropically dried with toluene (2×10 ml)
  4. additionThe residue was treated with 8% sodium bicarbonate solution (125 ml)
  5. extractionextracted with ethyl acetate (3×100 ml)
  6. filtrationThe combined extracts were filtered
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-17fb70c0ec7743a3875a61c35adcfdf8
출처 데이터셋
uspto-grants-1993_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05183820

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