Dichloromethane → 3-Acetylamino-5-amino-8-chloro-2,3-dihydroquinoline-4-one

HRID 1683493ノート

反応式

HRID 1683493 の反応式
[NH2:1][CH:2]1[C:11](=[O:12])[C:10]2[C:5](=[C:6]([Cl:14])[CH:7]=[CH:8][C:9]=2[NH2:13])[NH:4][CH2:3]1.ClCCl.C1C[O:21][CH2:20][CH2:19]1.C(OC(=O)C)(=O)C>N1C=CC=CC=1>[C:20]([NH:1][CH:2]1[C:11](=[O:12])[C:10]2[C:5](=[C:6]([Cl:14])[CH:7]=[CH:8][C:9]=2[NH2:13])[NH:4][CH2:3]1)(=[O:21])[CH3:19]

参加物

6

反応物 4

HCID 6344DichloromethaneHCID 7918Acetic AnhydrideHCID 8028TetrahydrofuranHCID 224495153,5-Diamino-8-chloro-2,3-dihydro-quinoline-4-one

生成物 1

HCID 224495543-Acetylamino-5-amino-8-chloro-2,3-dihydroquinoline-4-one

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

260 mg of the compound prepared in (3) above was dissolved into a mixed solvent of 5 ml of dichloromethane and 5 ml of THF. To this solution were added 0.16 ml of pyridine and 0.13 ml of acetic anhydride while stirring under ice cooling, and the mixture was stirred for 20 minutes. The reaction product was concentrated, and after the addition of chloroform, the residue was washed with saturated sodium bicarbonate and saturated brine, and dried over anhydrous sodium sulfate. The product was concentrated and the residue was charged into ether and petroleum ether in to produce 287 mg powder of the title compound.

後処理

  1. stirringthe mixture was stirred for 20 minutes
  2. concentrationThe reaction product was concentrated
  3. additionafter the addition of chloroform
  4. washthe residue was washed with saturated sodium bicarbonate and saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationThe product was concentrated
  7. additionthe residue was charged into ether and petroleum ether in

出典と根拠

ORDレコード
ord-5422f91076ff4108a2e24140e503718c
出典データセット
uspto-grants-1997_06
特許番号
US05637770

反応ノート

読み込み中…