Acetic Acid → HCID 19035986, 화합물

HRID 263903노트

반응식

HRID 263903 반응식
Cl[CH:2]1[C:14]2[NH:13][C:12](=[O:15])[C:11](=[O:16])[NH:10][C:9]=2[C:8]2[CH:7]=[CH:6][CH:5]=[CH:4][C:3]1=2.[C:17]([OH:20])(=[O:19])[CH3:18]>>[C:17]([O:20][CH:2]1[C:14]2[NH:13][C:12](=[O:15])[C:11](=[O:16])[NH:10][C:9]=2[C:8]2[CH:7]=[CH:6][CH:5]=[CH:4][C:3]1=2)(=[O:19])[CH3:18]

참가 물질

3

반응물 2

HCID 176Acetic AcidHCID 19035982HCID 19035982, 화합물

생성물 1

HCID 19035986HCID 19035986, 화합물수율 57.5%

실험 절차

9-Chloro-9H-indeno[1,2-b]pyrazine-2,3(1H,4H)-dione (0.30 g, 1.28 mmol) was refluxed in 50 ml of acetic acid for 10 min. Activated carbon (100 mg) was added and the reaction mixture was filtered and evaporated in vacuo to about 3 ml, and 20 ml of water was added. The precipitate was filtered off and washed with water and dried to give 229 mg of the crude compound, which was recrystallized from acetic acid-water to yield 190 mg (57.5%) of the title compound. M.p.>300° C. 1H-NMR (DMSO-d6, δ): 2.13 (s, 3H), 6.36 (s, 1H), 7.15 (t, 1H), 7.29 (d, 1H) 7.35 (t, 1H), 7.5 (d, 1H), 12.0 (s, 1H), 12.4 (s, 1H).

후처리

  1. additionActivated carbon (100 mg) was added
  2. filtrationthe reaction mixture was filtered
  3. customevaporated in vacuo to about 3 ml, and 20 ml of water
  4. additionwas added
  5. filtrationThe precipitate was filtered off
  6. washwashed with water
  7. customdried
  8. customto give 229 mg of the crude compound, which
  9. customwas recrystallized from acetic acid-water

출처 및 근거

ORD 기록
ord-ad6eb70e97de4e0687da9a0c5f56fb44
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05646146

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