Potassium Cyanide → HCID 66989070、化合物

HRID 2407764ノート

反応式

HRID 2407764 の反応式
Br[C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[C:4]([O:11][CH2:12][CH3:13])[N:3]=1.[C-:14]#[N:15].[K+]>CN(C)C=O>[CH2:12]([O:11][C:4]1[N:3]=[C:2]([C:14]#[N:15])[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=1)[CH3:13]

参加物

4

反応物 2

HCID 9032Potassium CyanideHCID 8172142-bromo-6-ethoxy-3-nitropyridine

生成物 1

HCID 66989070HCID 66989070、化合物収率 38.7%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

To a solution of the compound prepared in Example 279 (0.317 g) in N,N-dimethylformamide (6 mL) was added potassium cyanide (0.100 g) at room temperature. The mixture was heated at 80° C. for 18 hours and then cooled to room temperature. The solids were filtered, and the filtrate diluted with ethyl acetate, washed with 1N hydrochloric acid and water. The organic layer was filtered, evaporated in vacuo and purified by column chromatography on silica gel (10-50% ethyl acetate in hexane) to obtain the title compound (0.096 g) having the following physical data.

後処理

  1. temperaturecooled to room temperature
  2. filtrationThe solids were filtered
  3. additionthe filtrate diluted with ethyl acetate
  4. washwashed with 1N hydrochloric acid and water
  5. filtrationThe organic layer was filtered
  6. customevaporated in vacuo
  7. custompurified by column chromatography on silica gel (10-50% ethyl acetate in hexane)

出典と根拠

ORDレコード
ord-65af8d9478df47698328469f64d40e7e
出典データセット
uspto-grants-2014_08
特許番号
US08809538B2

反応ノート

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