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Ammonia → Elpetrigine

HRID 1358968
ノート
印刷プレビュー

反応式

HRID 1358968 の反応式
[NH2:1][C:2]1[C:7]([C:8]2[CH:13]=[C:12]([Cl:14])[CH:11]=[C:10]([Cl:15])[C:9]=2[Cl:16])=[N:6][CH:5]=[C:4](Cl)[N:3]=1.[NH3:18]>C(O)C>[NH2:1][C:2]1[C:7]([C:8]2[CH:13]=[C:12]([Cl:14])[CH:11]=[C:10]([Cl:15])[C:9]=2[Cl:16])=[N:6][CH:5]=[C:4]([NH2:18])[N:3]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 222AmmoniaHCID 10990505HCID 10990505、化合物

生成物 1

HCID 9926001Elpetrigine

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
180 °C

実験手順

A suspension of 2-amino-6-chloro-3-(2,3,5-trichlorophenyl)pyrazine (0.3 g, 9.71×10−4 mole) in absolute ethanol (4 ml) and 0.880 aqueous ammonia (8.24 ml) was stirred and heated in an autoclave at 180° C. for 44 hrs The cooled mixture was evaporated in vacuo, and the residue extracted with chloroform (3×30 ml). The combined chloroform extracts were dried over anhydrous magnesium sulphate, filtered and the filtrate evaporated down in vacuo. The residue was purified by ‘flash chromatography’ using chloroform to 98:2 chloroform:methanol as the eluent. The product was triturated with 40-60° C. petroleum ether, filtered and dried in vacuo. Yield 0.155 g (56%), M.p. 178-180° C.

後処理

  1. customwas evaporated in vacuo
  2. extractionthe residue extracted with chloroform (3×30 ml)
  3. dry with materialThe combined chloroform extracts were dried over anhydrous magnesium sulphate
  4. filtrationfiltered
  5. customthe filtrate evaporated down in vacuo
  6. customThe residue was purified by ‘flash chromatography’
  7. customThe product was triturated with 40-60° C. petroleum ether
  8. filtrationfiltered
  9. customdried in vacuo

出典と根拠

ORDレコード
ord-61690103a7a64066b531e8fb1e886290
出典データセット
uspto-grants-2003_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06599905B2

反応ノート

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