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HCID 3042017、化合物 → HCID 18919350、化合物

HRID 1290815
ノート
印刷プレビュー

反応式

HRID 1290815 の反応式
[Cl:1][CH:2]=[CH:3][C:4](=O)[CH2:5]Cl.ClC=CC(=O)C(C)C.[NH2:16][C:17]1[N:21]=[CH:20][NH:19][N:18]=1>C(O)(=O)C>[Cl:1][CH2:2][C:3]1[N:18]2[N:19]=[CH:20][N:21]=[C:17]2[N:16]=[CH:5][CH:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 3042017HCID 3042017、化合物HCID 53421801HCID 53421801、化合物HCID 178418311HCID 178418311、化合物

生成物 1

HCID 18919350HCID 18919350、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

1,4-Dichloro-1-buten-3-one (10.9 g) (prepared in a manner analogous to the preparation of 1-chloro-4-methyl-1-penten-3-one described in Example 20 below), 3-amino-1,2,4-triazole (6.5 g) and glacial acetic acid were heated under reflux for 1 hour and 30 minutes. The reaction mixture was poured onto ice and extracted with dichloromethane. The organic layer was dried over magnesium sulphate and the solvent was evaporated to give a solid. The crude product was purified by flash chromatography using as eluent a mixture of dichloromethane and ethanol (in the ratio 97:3 respectively), followed by recrystallisation from tetrachloromethane, to give 7-chloromethyl-1,2,4-triazolo[1,5-a]pyrimidine. Yield 10.15 g.

後処理

  1. temperaturewere heated
  2. temperatureunder reflux for 1 hour and 30 minutes
  3. additionThe reaction mixture was poured onto ice
  4. extractionextracted with dichloromethane
  5. dry with materialThe organic layer was dried over magnesium sulphate
  6. customthe solvent was evaporated
  7. customto give a solid
  8. customThe crude product was purified by flash chromatography
  9. additiona mixture of dichloromethane and ethanol (in the ratio 97:3 respectively),
  10. customfollowed by recrystallisation from tetrachloromethane

出典と根拠

ORDレコード
ord-026c8a65562c4e2b93e9ac28749e2220
出典データセット
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05753665

反応ノート

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