Potassium Iodide → HCID 22508626, 화합물

HRID 458619

반응식

HRID 458619 반응식
[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

참가 물질

8

반응물 4

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

생성물 1

HCID 22508626HCID 22508626, 화합물

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-7334a02c700b42bdb9c1f534b68ac804
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07192952B2

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