Oxalic Acid → 6-Bromo-8-methyl-1,4,7,8,9,10-hexahydro-pyrido[4,3-f]quinoxaline-2,3-dione

HRID 48207노트

반응식

HRID 48207 반응식
[Br:1][C:2]1[CH:3]=[C:4]([NH2:14])[C:5]([NH2:13])=[C:6]2[C:11]=1[CH2:10][N:9]([CH3:12])[CH2:8][CH2:7]2.[C:15](O)(=[O:19])[C:16](O)=[O:17]>Cl>[Br:1][C:2]1[C:11]2[CH2:10][N:9]([CH3:12])[CH2:8][CH2:7][C:6]=2[C:5]2[NH:13][C:15](=[O:19])[C:16](=[O:17])[NH:14][C:4]=2[CH:3]=1

참가 물질

4

반응물 2

HCID 971Oxalic AcidHCID 103550328-Bromo-1,2,3,4-tetrahydro-2-methyl-5,6-isoquinolinediamine

생성물 1

HCID 98181346-Bromo-8-methyl-1,4,7,8,9,10-hexahydro-pyrido[4,3-f]quinoxaline-2,3-dione수율 24.1%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

A solution of the product from Example 13 (0.62 g, 2.56 mmol) and oxalic acid (0.23 g, 2.56 mmol) in 25 mL of 3N aqueous HCl solution were heated at reflux for 18 hours. The reaction mixture was cooled to room temperature and the solid which formed was collected by filtration and washed with cold water. The solid was recrystallized from hot water and dried under vacuum (100° C., P2O5) to give the title compound as a tan solid (0.191 g, 20%), mp=315-320° C. (dec.).

후처리

  1. temperatureat reflux for 18 hours
  2. customthe solid which formed
  3. filtrationwas collected by filtration
  4. washwashed with cold water
  5. customThe solid was recrystallized from hot water
  6. dry with materialdried under vacuum (100° C., P2O5)

출처 및 근거

ORD 기록
ord-28485785eeb5490989bcf2076b9474c3
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06703391B2

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