Tin atom → 7-Phenyl-1H-pyrido[2,3-b][1,4]oxazin-2(3H)-one

HRID 1509273ノート

反応式

HRID 1509273 の反応式
[N+:1]([C:4]1[C:5]([O:16][CH2:17][C:18]([O:20]CC)=O)=[N:6][CH:7]=[C:8]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH:9]=1)([O-])=O.[Sn]>Cl>[C:10]1([C:8]2[CH:7]=[N:6][C:5]3[O:16][CH2:17][C:18](=[O:20])[NH:1][C:4]=3[CH:9]=2)[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

参加物

4

反応物 2

HCID 5352426Tin atomHCID 67255179Ethyl 2-((3-nitro-5-phenylpyridin-2-yl)oxy)acetate

生成物 1

HCID 669367437-Phenyl-1H-pyrido[2,3-b][1,4]oxazin-2(3H)-one

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

反応条件

温度
2.5 °C

実験手順

In a 500 ml round-bottomed flask was added ethyl 2-(3-nitro-5-phenylpyridin-2-yloxy)acetate (4.6 g, 15.22 mmol) in hydrochloric acid, 37% (40 ml) to give a yellow suspension. The mixture was cooled to 0-5° C. followed by the portion wise addition of tin powder (9.94 g, 84 mmol). The addition proved to be exothermic. Caution should be taken while adding. The mixture was then stirred at room temperature for further 30 minutes until all foaming ceased. The reaction mixture was heated to 80° C. under a nitrogen atmosphere for 3 hours.

後処理

  1. customto give a yellow suspension
  2. additionThe addition
  3. additionwhile adding
  4. temperatureThe reaction mixture was heated to 80° C. under a nitrogen atmosphere for 3 hours

出典と根拠

ORDレコード
ord-f13cf9e9ce16442abb54db50a4d6fd1e
出典データセット
uspto-grants-2015_12
特許番号
US09221838B2

反応ノート

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