Methane → 10-amino-10-methyl-5H,10H-imidazo[1,2-a]indeno[1,2-e]-pyrazin-4-one hydrochloride

HRID 2393383노트

반응식

HRID 2393383 반응식
C([NH:4][C:5]1([CH3:22])[C:17]2[N:16]3[CH:18]=[CH:19][N:20]=[C:15]3[C:14](=[O:21])[NH:13][C:12]=2[C:11]2[CH:10]=[CH:9][CH:8]=[CH:7][C:6]1=2)(=O)C.C.[ClH:24]>CO>[ClH:24].[NH2:4][C:5]1([CH3:22])[C:17]2[N:16]3[CH:18]=[CH:19][N:20]=[C:15]3[C:14](=[O:21])[NH:13][C:12]=2[C:11]2[CH:10]=[CH:9][CH:8]=[CH:7][C:6]1=2

참가 물질

5

반응물 3

HCID 297MethaneHCID 313Hydrochloric AcidHCID 1897538710-acetamido-10-methyl-5H,10H-imidazo[1,2-a]indeno[1,2-e]pyrazin-4-one

생성물 1

HCID 1897542610-amino-10-methyl-5H,10H-imidazo[1,2-a]indeno[1,2-e]-pyrazin-4-one hydrochloride

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A suspension of 1 g of 10-acetamido-10-methyl-5H,10H-imidazo[1,2-a]indeno[1,2-e]pyrazin-4-one in 50 ml of 2N hydrochloric acid is boiled for 1 hour 45 minutes and the solution obtained is concentrated to dryness under reduced pressure (1 mmHg; 0.13 kPa) at 70° C. The product obtained (1.15 g) is dissolved in 100 ml of methanol and, after addition of decolorizing charcoal, the solution is filtered. 300 ml of acetone are added and, after storing for 1 hour at 5° C., the solid formed is isolated by filtration, washed twice with 10 ml in total of chilled acetone and dried under reduced pressure (1 mmHg; 0.13 kPa) at 100° C. 0.39 g of 10-amino-10-methyl-5H,10H-imidazo[1,2-a]indeno[1,2-e]-pyrazin-4-one hydrochloride is thus obtained, decomposing without melting above 260° C. (NMR spectrum: [200 MHz; (CD3)2SO-d6 ; δ in ppm]: 1.97 (s, 3H: --CH3 at 10); 7.48 and 7.55 (2t, J=7.5 Hz, 1H each: --H 7 and --H 8); 7.70 and 8.75 (2 broad s, 1H each: --H of the imidazole); 7.95 and 8.08 (2d, J=7.5 Hz, 1H each: --H 6 and --H 9); 9.39 (mult., 3H: --NH3+Cl- at 10); 12.64 (mult., 1H: --NHCO--)).

후처리

  1. customthe solution obtained
  2. concentrationis concentrated to dryness under reduced pressure (1 mmHg; 0.13 kPa) at 70° C
  3. customThe product obtained (1.15 g)
  4. filtrationthe solution is filtered
  5. addition300 ml of acetone are added
  6. waitafter storing for 1 hour at 5° C.
  7. customthe solid formed
  8. customis isolated by filtration
  9. washwashed twice with 10 ml in total of chilled acetone
  10. customdried under reduced pressure (1 mmHg; 0.13 kPa) at 100° C

출처 및 근거

ORD 기록
ord-37b29d14f3bc43899b07e318c0c44ff0
출처 데이터셋
uspto-grants-1998_09
특허 번호
US05807859

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