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Phosphorus pentachloride → 4-Chloro-2-(1-methyl-5-nitro-1H-imidazol-2-yl)quinazoline

HRID 973209
ノート
印刷プレビュー

反応式

HRID 973209 の反応式
[CH3:1][N:2]1[C:6]([N+:7]([O-:9])=[O:8])=[CH:5][N:4]=[C:3]1[C:10]1[NH:19][C:18](=O)[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[N:11]=1.P(Cl)(Cl)(Cl)(Cl)[Cl:22]>P(Cl)(Cl)(Cl)=O>[CH3:1][N:2]1[C:6]([N+:7]([O-:9])=[O:8])=[CH:5][N:4]=[C:3]1[C:10]1[N:19]=[C:18]([Cl:22])[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[N:11]=1
参加物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 24819Phosphorus pentachlorideHCID 1357273912-(1-Methyl-5-nitro-1H-imidazol-2-yl)quinazolin-4(1H)-one

生成物 1

HCID 214020964-Chloro-2-(1-methyl-5-nitro-1H-imidazol-2-yl)quinazoline

試薬・触媒・溶媒 1

HCID 24813Phosphorus oxychloride溶媒

実験手順

A suspension of 25 g of 2-(1-methyl-5-nitro-2-imidazolyl)-4-quinazolinone and 26.2 g of phosphorus pentachloride in 150 ml of phosphorus oxychloride is boiled for 3 hours and then evaporated in vacuo (12 Torr). The residue is taken up in methylene chloride and stirred with water for one hour at room temperature. The mixture is made alkaline with sodium bicarbonate and extracted by dropwise addition of methylene chloride. The mixture is dried with magnesium sulphate and treated with animal charcoal, filtered and evaporated in vacuo (12 Torr) at 30° C. The residue is mixed with ether, filtered and washed pure with ether to obtain the heading compound, m.p. 178°-181° C.

後処理

  1. customevaporated in vacuo (12 Torr)
  2. extractionextracted by dropwise addition of methylene chloride
  3. dry with materialThe mixture is dried with magnesium sulphate
  4. additiontreated with animal charcoal
  5. filtrationfiltered
  6. customevaporated in vacuo (12 Torr) at 30° C
  7. additionThe residue is mixed with ether
  8. filtrationfiltered
  9. washwashed pure with ether
  10. customto obtain the heading compound, m.p. 178°-181° C.

出典と根拠

ORDレコード
ord-62279d4f02cf488fb8b4a6ae26723e95
出典データセット
uspto-grants-1977_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04055642

反応ノート

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