Benzene → HCID 19772346、化合物

HRID 1463535ノート

反応式

HRID 1463535 の反応式
[C:1]1([C:7]2[C:12]3[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=3[CH2:10][S:9][C:8]=2C(O)=O)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C1C=CC(P(N=[N+]=[N-])(C2C=CC=CC=2)=[O:27])=CC=1.C1C=CC=CC=1.Cl.[C:44]([O:47][C:48]1[C:54]([CH3:55])=[CH:53][C:51]([NH2:52])=[CH:50][C:49]=1[CH3:56])(=[O:46])[CH3:45].C([N:59]([CH2:62]C)CC)C>>[C:44]([O:47][C:48]1[C:54]([CH3:55])=[CH:53][C:51]([NH:52][C:62]([NH:59][C:8]2[S:9][CH2:10][C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[C:7]=2[C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)=[O:27])=[CH:50][C:49]=1[CH3:56])(=[O:46])[CH3:45]

参加物

6

反応物 5

HCID 241BenzeneHCID 8471TriethylamineHCID 199401P,P-Diphenylphosphinic azideHCID 19090525HCID 19090525、化合物HCID 19090551HCID 19090551、化合物

生成物 1

HCID 19772346HCID 19772346、化合物

実験手順

To a mixture of 4-phenyl-1H-2-benzothiopyran-3-carboxylic acid (in Reference Example 13) (268 mg), DPPA (330 mg) and benzene (5 ml) was added dropwise to triethylamime (0.14 ml) and the mixture was stirred at room temperature for 30 minutes, then refluxed for 30 minutes. To the mixture were added 4-acetoxy-3,5-dimethylaniline hydrochloride (258 mg) and triethylamine (0.17 ml), followed by refluxing for 20 minutes. The mixture was washed with water, then dried (MgSO4), followed by distilling off the solvent. To the residue was added ether to afford the above-titled compound as colorless crystals (280 mg).

後処理

  1. additionwas added dropwise to triethylamime (0.14 ml)
  2. temperaturerefluxed for 30 minutes
  3. temperatureby refluxing for 20 minutes
  4. washThe mixture was washed with water
  5. dry with materialdried (MgSO4)
  6. distillationby distilling off the solvent
  7. additionTo the residue was added ether

出典と根拠

ORDレコード
ord-e395a4606132456aa4f369f795be6d0e
出典データセット
uspto-grants-1994_04
特許番号
US05300646

反応ノート

読み込み中…