Isopropyl iodide → 7-[4-(4-Chlorobenzoyl)benzyl]-1-isopropyl-3-methylxanthine

HRID 1291412

반응식

HRID 1291412 반응식
[CH3:1][N:2]1[C:10]2[N:9]=[CH:8][N:7]([CH2:11][C:12]3[CH:17]=[CH:16][C:15]([C:18](=[O:26])[C:19]4[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][CH:20]=4)=[CH:14][CH:13]=3)[C:6]=2[C:5](=[O:27])[NH:4][C:3]1=[O:28].C(=O)([O-])[O-].[K+].[K+].[CH:35](I)([CH3:37])[CH3:36]>CN(C=O)C.O>[Cl:25][C:22]1[CH:23]=[CH:24][C:19]([C:18]([C:15]2[CH:14]=[CH:13][C:12]([CH2:11][N:7]3[C:6]4[C:5](=[O:27])[N:4]([CH:35]([CH3:37])[CH3:36])[C:3](=[O:28])[N:2]([CH3:1])[C:10]=4[N:9]=[CH:8]3)=[CH:17][CH:16]=2)=[O:26])=[CH:20][CH:21]=1

참가 물질

6

반응물 3

HCID 6362Isopropyl iodideHCID 11430Potassium CarbonateHCID 189188013-Methyl-7-[4-(4-chlorobenzoyl)benzyl]xanthine

생성물 1

HCID 189192457-[4-(4-Chlorobenzoyl)benzyl]-1-isopropyl-3-methylxanthine수율 6.3%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

A solution of 3-methyl-7-[4-(4-chlorobenzoyl)-benzyl]xanthine (544 mg), potassium carbonate (202 mg) and isopropyl iodide (356 mg) in DMF (10 ml) was stirred at 60° C. for 5 hours. This reaction mixture was poured in water and extracted with ethyl acetate. The extract was washed with water, dried and concentrated. The residue was purified by silica gel column chromatography (hexane: ethyl acetate =1:1) and recrystallized from acetone-hexane to provide the title compound as colorless solid (38 mg).

후처리

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with water
  3. customdried
  4. concentrationconcentrated
  5. customThe residue was purified by silica gel column chromatography (hexane: ethyl acetate =1:1)
  6. customrecrystallized from acetone-hexane

출처 및 근거

ORD 기록
ord-bcf7b3611c324a34a886238f54b510c8
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05753664

연결된 노트

불러오는 중…