Semicarbazide hydrochloride → HCID 178510553, 화합물

HRID 240325노트

반응식

HRID 240325 반응식
[Cl:1][C:2]1[CH:18]=[CH:17][C:16]2[C:7]3=[N:8][C:9]([C:14]#[N:15])=[C:10]([C:12]#[N:13])[N:11]=[C:6]3[C:5](=O)[C:4]=2[CH:3]=1.Cl.[NH2:21][NH:22][C:23]([NH2:25])=[O:24]>C(#N)C>[NH2:25][C:23]([NH:22][N:21]=[C:5]1[C:6]2[C:7](=[N:8][C:9]([C:14]#[N:15])=[C:10]([C:12]#[N:13])[N:11]=2)[C:16]2[CH:17]=[CH:18][C:2]([Cl:1])=[CH:3][C:4]1=2)=[O:24]

참가 물질

4

반응물 2

HCID 11236Semicarbazide hydrochlorideHCID 160657737-Chloro-9-oxo-9H-indeno[1,2-b]pyrazine-2,3-dicarbonitrile

생성물 1

HCID 178510553HCID 178510553, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A mixture of 600 mg (2.25 mmol) 17g and 329 mg (2.92 mmol) semicarbazide hydrochloride in 20 ml acetonitrile was heated 14 h under reflux. After that time, TLC indicated complete conversion of the starting product. After evaporation of the solvent, the crude product was recrystallised from aqueous ethanol, and compound 43 was obtained in slightly greenish crystals (90%). 1H-NMR (d6-DMSO, 400 MHz): δ (ppm)=7.40 (sl, 1H); 7.70 (sl, 1H); 7.71 (d, J=8 Hz, 1H); 8.17 (d, J=8 Hz, 1H); 8.89 (s, 1H); 10.95 (s, 1H). ESI+MS: calcd for C14H6ClN7O: 323.70; found: 324 (MH+).

후처리

  1. temperaturewas heated 14 h
  2. temperatureunder reflux
  3. customAfter evaporation of the solvent
  4. customthe crude product was recrystallised from aqueous ethanol

출처 및 근거

ORD 기록
ord-dcc7dd220a3f4b4b97eec03beb8417d4
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08648076B2

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