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

HRID 1106426노트

반응식

HRID 1106426 반응식
[Br:1][C:2]1[CH:11]=[C:10]([NH2:12])[C:9]([NH2:13])=[C:8]2[C:3]=1[CH2:4][CH2:5][N:6]([CH2:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[CH2:7]2.[C:21](O)(=[O:25])[C:22](O)=[O:23]>Cl>[Br:1][C:2]1[C:3]2[CH2:4][CH2:5][N:6]([CH2:14][C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)[CH2:7][C:8]=2[C:9]2[NH:13][C:21](=[O:25])[C:22](=[O:23])[NH:12][C:10]=2[CH:11]=1

참가 물질

4

반응물 2

HCID 971Oxalic AcidHCID 155241895-Bromo-1,2,3,4-tetrahydro-2-(phenylmethyl)-7,8-isoquinolinediamine

생성물 1

HCID 155241906-Bromo-1,4,7,8,9,10-hexahydro-9-(phenylmethyl)pyrido[3,4-f]quinoxaline-2,3-dione수율 89%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

A solution of the product from Example 7 (0.64 g, 1.93 mmol) in 3N HCl (25 mL) was treated with oxalic acid (0.37 g, 2.9 mmol) and refluxed for four hours. When cool to room temperature the precipitate was filtered, suspended in water (70 mL) and basifyed to pH 10. The solids were filtered, and dried to give the title compound (0.57 g, 89%) as a light brown solid, mp=297-302° C.

후처리

  1. temperaturerefluxed for four hours
  2. filtrationwas filtered
  3. filtrationThe solids were filtered
  4. customdried

출처 및 근거

ORD 기록
ord-6b87b5aeaa6a49b2a322324572935068
출처 데이터셋
uspto-grants-2000_05
특허 번호
US06057313

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