Potassium Iodide → HCID 22508626、化合物

HRID 458619

反応式

HRID 458619 の反応式
[Cl:1][C:2]1[NH:11][C:10]2[C:9](=[O:12])[N:7]([CH3:8])[C:6](=[O:13])[N:5]([CH3:14])[C:4]=2[N:3]=1.[I:15][C:16]1[CH:23]=[CH:22][CH:21]=[CH:20][C:17]=1[CH2:18]Cl.C(=O)([O-])[O-].[K+].[K+].[I-].[K+]>CN(C=O)C.CCOC(C)=O.O>[Cl:1][C:2]1[N:11]([CH2:18][C:17]2[CH:20]=[CH:21][CH:22]=[CH:23][C:16]=2[I:15])[C:10]2[C:9](=[O:12])[N:7]([CH3:8])[C:6](=[O:13])[N:5]([CH3:14])[C:4]=2[N:3]=1

参加物

8

反応物 4

HCID 4875Potassium IodideHCID 106618-ChlorotheophyllineHCID 11430Potassium CarbonateHCID 1010641-(Chloromethyl)-2-iodobenzene

生成物 1

HCID 22508626HCID 22508626、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

8-Chlorotheophylline (8.5 g, 39.6 mmol) was dissolved in 400 ml of DMF and 2-iodobenzyl chloride (10.0 g, 39.6 mmol), potassium carbonate (5.47 g, 39.6 mmol), and potassium iodide (10 mg, 0.06 mmol) were added. The mixture was stirred at room temperature for 7 days. Water (2500 ml) and EtOAc (800 ml) were added and the layers were separated. The aqueous layer was extracted with 2×500 ml of EtOAc, and the combined organic layer was washed with 500 ml of water, 500 ml of brine, dried over sodium sulphate, and filtered. The solvent was evaporated and the crude product was crystallized from diethyl ether and petrol, to give compound (5A) as white crystals. The mother liquor was evaporated and resuspended in diethyl ether and petrol, to give a second crop of compound (5A).

後処理

  1. customthe layers were separated
  2. extractionThe aqueous layer was extracted with 2×500 ml of EtOAc
  3. washthe combined organic layer was washed with 500 ml of water, 500 ml of brine
  4. dry with materialdried over sodium sulphate
  5. filtrationfiltered
  6. customThe solvent was evaporated
  7. customthe crude product was crystallized from diethyl ether and petrol

出典と根拠

ORDレコード
ord-7334a02c700b42bdb9c1f534b68ac804
出典データセット
uspto-grants-2007_03
特許番号
US07192952B2

関連ノート

読み込み中…