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Oxalic acid dihydrate → HCID 19827847, 화합물

HRID 1494324
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HRID 1494324 반응식
[CH2:1]([NH:8][C:9]1[CH:14]=[CH:13][C:12]([N+:15]([O-:17])=[O:16])=[CH:11][C:10]=1[NH2:18])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.O.[C:21](O)(=[O:25])[C:22](O)=[O:23]>Cl>[CH2:1]([N:8]1[C:9]2[C:10](=[CH:11][C:12]([N+:15]([O-:17])=[O:16])=[CH:13][CH:14]=2)[NH:18][C:22](=[O:23])[C:21]1=[O:25])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 61373Oxalic acid dihydrateHCID 4381698N~1~-benzyl-4-nitro-1,2-benzenediamine

생성물 1

HCID 19827847HCID 19827847, 화합물수율 49%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

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온도
25 °C

실험 절차

A mixture of 0.5 g (2.1 mmol) N-benzyl-2-amino-4-nitroaniline and 0.55 g (4.4 mmol) oxalic acid dihydrate in 30 ml 4N hydrochloric acid was refluxed for 5 h. After cooling to 25° C. the product was filtered off and washed with water. The crude product was recrystallized (dimethylformamide-water), washed with 10 ml water, 5 ml ethanol and 5 ml ether to give 0.3 g (49%) 1-benzyl-6-nitroquinoxaline-2,3(1H,4H)-dione. M.p. (DSC): 292.2° C. 1H-NMR (DMSO-d6): 12.4 (1H, broad s), 8.2-7.0 (8H, m), 5.4 (2H, s).

후처리

  1. temperaturewas refluxed for 5 h
  2. filtrationwas filtered off
  3. washwashed with water
  4. customThe crude product was recrystallized (dimethylformamide-water)
  5. washwashed with 10 ml water, 5 ml ethanol and 5 ml ether

출처 및 근거

ORD 기록
ord-154b1c34f6774ceb9f431f719fa3ddad
출처 데이터셋
uspto-grants-1991_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05026704

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