Stannous chloride dihydrate → 7-Chloro-3,4-dihydro-6-methyl-2(1H)-quinoxalinone

HRID 1781008노트

반응식

HRID 1781008 반응식
[Na+].[Cl:2][C:3]1[C:8]([CH3:9])=[CH:7][C:6]([NH:10][CH2:11][C:12]([O-])=[O:13])=[C:5]([N+:15]([O-])=O)[CH:4]=1.O.O.[Sn](Cl)Cl>C(O)C>[Cl:2][C:3]1[CH:4]=[C:5]2[C:6]([NH:10][CH2:11][C:12](=[O:13])[NH:15]2)=[CH:7][C:8]=1[CH3:9]

참가 물질

4

반응물 2

HCID 61436Stannous chloride dihydrateHCID 21189951HCID 21189951, 화합물

생성물 1

HCID 100814077-Chloro-3,4-dihydro-6-methyl-2(1H)-quinoxalinone수율 66.2%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of N-(4'-chloro-5'-methyl-2'-nitrophenyl)glycine sodium salt (0.300 g, 1.23 mmol, as prepared above) and tin (II) chloride dihydrate (0.830 g, 3.68 mmol, Aldrich, used as received) in ethanol (4.0 mL) was refluxed for 30 min. It was then cooled to room temperature and the precipitated solid was filtered, washed with ethanol (1.0 mL) and dried under vacuum to yield 0.160 g (66%) of the title compound as a yellow powder; 1H NMR (DMSO-d6): δ2.099 (s, 3H), 3.655 (s, 2H), 6.037 (s, 1H), 6.538 (s, 1H), 6.685 (s, 1H), 10.241 (s, 1H).

후처리

  1. filtrationthe precipitated solid was filtered
  2. washwashed with ethanol (1.0 mL)
  3. customdried under vacuum

출처 및 근거

ORD 기록
ord-cddbda38d6b149dc93731d7fe0f4c254
출처 데이터셋
uspto-grants-1997_05
특허 번호
US05631373

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