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

HRID 499566

反応式

HRID 499566 の反応式
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]

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d2ceec83bc854dd18583a6682f2a90d1
出典データセット
uspto-grants-2010_08
特許番号
US07767665B2

関連ノート

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