4-Carbamoyl-1-(2,4-dinitrophenyl)pyridinium chloride → HCID 10540454、化合物

HRID 964011ノート

反応式

HRID 964011 の反応式
[O:1]1[CH2:5][CH2:4][C:3]2[CH:6]=[CH:7][CH:8]=[C:9]([NH2:10])[C:2]1=2.[Cl-:11].[C:12]([C:15]1[CH:20]=[CH:19][N+](C2C=CC([N+]([O-])=O)=CC=2[N+]([O-])=O)=[CH:17][CH:16]=1)(=[O:14])[NH2:13]>CO>[Cl-:11].[O:1]1[CH2:5][CH2:4][C:3]2[CH:6]=[CH:7][CH:8]=[C:9]([N+:10]3[CH:19]=[CH:20][C:15]([C:12](=[O:14])[NH2:13])=[CH:16][CH:17]=3)[C:2]1=2

参加物

4

反応物 2

HCID 106160034-Carbamoyl-1-(2,4-dinitrophenyl)pyridinium chlorideHCID 128059502,3-Dihydro-1-benzofuran-7-amine

生成物 1

HCID 10540454HCID 10540454、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of 2,3-dihydrobenzo[b]furan-7-ylamine (6.8 g prepared in a similar manner to that described in Tetrahedron Letters 1982,23,147), 4-carbamoyl-1-(2,4-dinitrophenyl)pyridinium chloride (14.7 g prepared in a similar manner to that described in Example 2) and methanol (400 ml) was stirred under reflux for 5 hours then allowed to stand at ambient temperature and heated for 16 hours. The solvent was removed in vacuo, and the residue was triturated with hot acetone, cooled and filtered to give 1-(2,3-dihydrobenzo[b]furan-7-yl)-4-carbamoylpyridinium chloride as a yellow solid (11.5 g), m.p. 289°-290° C.

後処理

  1. customprepared in a similar manner to that
  2. customprepared in a similar manner to that
  3. temperatureunder reflux for 5 hours
  4. customto stand at ambient temperature
  5. temperatureheated for 16 hours
  6. customThe solvent was removed in vacuo
  7. customthe residue was triturated with hot acetone
  8. temperaturecooled
  9. filtrationfiltered

出典と根拠

ORDレコード
ord-0fc4e65ccaaa485c857668d0d2669af8
出典データセット
uspto-grants-1998_06
特許番号
US05767116

反応ノート

読み込み中…