Hydroxyamine hydrochloride → HCID 178516735, 화합물

HRID 129443노트

반응식

HRID 129443 반응식
[N:1]1[C:2]2[C:14](=O)[C:13]3[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=3[C:3]=2[NH:4][C:5](=[O:7])[CH:6]=1.Cl.[NH2:17][OH:18]>N1C=CC=CC=1>[OH:18][N:17]=[C:14]1[C:2]2[N:1]=[CH:6][C:5](=[O:7])[NH:4][C:3]=2[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:13]1=2

참가 물질

4

반응물 2

HCID 443297Hydroxyamine hydrochlorideHCID 190359769H-Indeno[1,2-b]pyrazine-3,9(4H)-dione

생성물 1

HCID 178516735HCID 178516735, 화합물수율 49%

시약·촉매·용매 1

HCID 1049Pyridine용매

반응 조건

온도
80 °C

실험 절차

A mixture of 9H-indeno[1,2-b]pyrazine-3,9(4H)-dione (1.0 g, 5.0 mmol), pyridine (40 ml) and hydroxylamine hydrochloride (0.42 g, 6.0 mmol) was stirred at 80° C. for 18 hours. The reaction mixture was cooled to room temperature, and the precipitate was filtered off and washed with water, acetic acid and water and dried. The crude material (0.81 g) was recrystallized from DMF to afford 0.52 g (49%) of the title compound. M.p. >300° C. 1H-NMR (DMSO-d6, δ): 7.49-7.62 (m, 2H), 7.88 (d, 1H), 7.95 (s, 1H), 8.36 (d, 1H), 12.5-13.2 (broad, 1H), 12.83 (s, 1H).

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. filtrationthe precipitate was filtered off
  3. washwashed with water, acetic acid and water
  4. customdried
  5. customThe crude material (0.81 g) was recrystallized from DMF

출처 및 근거

ORD 기록
ord-b2ba53c1c31a49e8888e0bd501cee82c
출처 데이터셋
uspto-grants-1995_11
특허 번호
US05468748

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