Phosphorus pentachloride → HCID 19902182、化合物

HRID 2372724ノート

反応式

HRID 2372724 の反応式
[N:1]1[CH2:2][CH2:3][N:4]2[C:13]=1[C:12]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[N:6]1[CH:14]=[N:15][C:16]([C:17]([NH2:19])=O)=[C:5]21.P(Cl)(Cl)(Cl)(Cl)Cl>P(Cl)(Cl)(Cl)=O>[C:17]([C:16]1[N:15]=[CH:14][N:6]2[C:7]3[CH:8]=[CH:9][CH:10]=[CH:11][C:12]=3[C:13]3=[N:1][CH2:2][CH2:3][N:4]3[C:5]=12)#[N:19]

参加物

4

反応物 2

HCID 24819Phosphorus pentachlorideHCID 19902191HCID 19902191、化合物

生成物 1

HCID 19902182HCID 19902182、化合物

試薬・触媒・溶媒 1

HCID 24813Phosphorus oxychloride溶媒

反応条件

温度
0 °C

実験手順

A mixture of 2,3-dihydrodiimidazo[1,5-a:1',2'-c]quinazoline-5-carboxamide (1 g, 4 mmol) (prepared by standard methods from the corresponding carboxylic acid ethyl ester, Compound 3) and phosphorus pentachloride (0.9 g, 4.1 mmol) in phosphorus oxychloride (10 ml) was stirred at reflux for 3 h, and then evaporated to dryness. The residue was partitioned between 25 ml of water and 25 ml of dichloromethane. The organic layer was extracted with 4×25 ml of 10% acetic acid. The combined aqueous phases were adjusted to pH around 11 and cooled to 0° C. The precipitate which had formed was filtered off and dried, giving the title compound as yellow crystals, m.p. 227°-240° C. (decomposition). Yield 0.53 g (57%). (Compound 49).

後処理

  1. temperatureat reflux for 3 h
  2. customevaporated to dryness
  3. customThe residue was partitioned between 25 ml of water and 25 ml of dichloromethane
  4. extractionThe organic layer was extracted with 4×25 ml of 10% acetic acid
  5. customThe precipitate which had formed
  6. filtrationwas filtered off
  7. customdried

出典と根拠

ORDレコード
ord-faf67c0f371246a496940f4f4be12afe
出典データセット
uspto-grants-1992_03
特許番号
US05100895

反応ノート

読み込み中…