1,4-Dioxane → 2-Amino-5-pyridin-3-ylthiophene-3-carbonitrile

HRID 386134ノート

反応式

HRID 386134 の反応式
C(OC(=O)[NH:7][C:8]1[S:9][C:10]([C:15]2[CH:16]=[N:17][CH:18]=[CH:19][CH:20]=2)=[CH:11][C:12]=1[C:13]#[N:14])(C)(C)C.O1CCOCC1>Cl>[NH2:7][C:8]1[S:9][C:10]([C:15]2[CH:16]=[N:17][CH:18]=[CH:19][CH:20]=2)=[CH:11][C:12]=1[C:13]#[N:14]

参加物

4

反応物 2

HCID 312751,4-DioxaneHCID 70842621HCID 70842621、化合物

生成物 1

HCID 686716452-Amino-5-pyridin-3-ylthiophene-3-carbonitrile

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

tert-Butyl(3-cyano-5-pyridin-3-yl-2-thienyl)carbamate (800 mg, 2.07 mmol) was dissolved in 4M hydrochloric acid in dioxane (10.4 ml, 41.6 mmol) and the mixture was stirred at room temperature for 6 h. The mixture was quenched with 1N sodium hydroxide (50 mL) and extracted with ethyl acetate (3×100 mL). The combined organics were dried over anhydrous magnesium sulfate, filtered, and concentrated under reduced pressure to afford the title compound as a solid.

後処理

  1. customThe mixture was quenched with 1N sodium hydroxide (50 mL)
  2. extractionextracted with ethyl acetate (3×100 mL)
  3. dry with materialThe combined organics were dried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-90de99c0f10a42e5893ee2e2ccc47b85
出典データセット
uspto-grants-2013_02
特許番号
US08367706B2

反応ノート

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