Sodium hydrosulfide → HCID 178418602、化合物

HRID 5816

反応式

HRID 5816 の反応式
Cl[C:2]1[CH:11]=[N:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.[SH-:12].[Na+]>CN(C)C=O>[SH:12][C:2]1[CH:11]=[N:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1

参加物

4

反応物 2

HCID 28015Sodium hydrosulfideHCID 2389382-Chloroquinoxaline

生成物 1

HCID 178418602HCID 178418602、化合物収率 157.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
100 °C

実験手順

2-Chloroquinoxaline (2 g) and sodium hydrosulphide (1.23 g) were stirred together in 25 ml of dimethylformamide and heated to 100° C. After 3 hours the reaction mixture was allowed to cool and then partitioned between 70 ml of water and 30 ml of ethyl acetate. The organic layer was separated and the aqueous layer extracted twice with 20 ml of ethyl acetate. The combined organic extracts were washed with sodium chloride solution, dried over anhydrous magnesium sulphate, filtered and the solvent removed under reduced pressure to yield an orange solid (3.1 g). The product of this reaction was used in the next preparative step without further purification.

後処理

  1. temperatureto cool
  2. custompartitioned between 70 ml of water and 30 ml of ethyl acetate
  3. customThe organic layer was separated
  4. extractionthe aqueous layer extracted twice with 20 ml of ethyl acetate
  5. washThe combined organic extracts were washed with sodium chloride solution
  6. dry with materialdried over anhydrous magnesium sulphate
  7. filtrationfiltered
  8. customthe solvent removed under reduced pressure

出典と根拠

ORDレコード
ord-774ce888c2ae4a3eb24f6b6510e760c5
出典データセット
uspto-grants-1993_09
特許番号
US05246933

関連ノート

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