Tetrahydrofuran → 2-Cyano-6-[2-(dimethylamino)ethylthio]pyrazine

HRID 499566

반응식

HRID 499566 반응식
Cl.[CH3:2][N:3]([CH3:7])[CH2:4][CH2:5][SH:6].[H-].[Na+].C1COCC1.Cl[C:16]1[CH:21]=[N:20][CH:19]=[C:18]([C:22]#[N:23])[N:17]=1>O.C(OCC)(=O)C>[C:22]([C:18]1[CH:19]=[N:20][CH:21]=[C:16]([S:6][CH2:5][CH2:4][N:3]([CH3:7])[CH3:2])[N:17]=1)#[N:23]

참가 물질

7

반응물 4

HCID 8028TetrahydrofuranHCID 24758Sodium hydrideHCID 25798Captamine HydrochlorideHCID 813036-Chloropyrazine-2-carbonitrile

생성물 1

HCID 229395352-Cyano-6-[2-(dimethylamino)ethylthio]pyrazine수율 48%

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

2-Dimethylaminoethanethiol hydrochloride salt (1.46 g, 10.0 mmol) and sodium hydride (60% in oil, 0.88 g, 22.0 mmol) were added to THF (50 ml), and 2-chloro-6-cyanopyrazine (1.40 g, 10.0 mmol) was added thereto. The mixture was stirred at room temperature for 18 hrs. The reaction mixture was combined with ethyl acetate and water. The organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated, and the residue was recrystallized from n-hexane-ethyl acetate to give the titled compound (1.00 g, 48%) as pale yellow crystals.

후처리

  1. additionwas added
  2. washThe organic layer was washed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was evaporated
  5. customthe residue was recrystallized from n-hexane-ethyl acetate

출처 및 근거

ORD 기록
ord-d2ceec83bc854dd18583a6682f2a90d1
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07767665B2

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