Water → 8-(3-Aminoazepan-1-yl)-7-(2-bromobenzyl)-3-methyl-3,7-dihydropurine-2,6-dione

HRID 458637

반응식

HRID 458637 반응식
Br[C:2]1[N:10]([CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=2[Br:18])[C:9]2[C:8](=[O:19])[NH:7][C:6](=[O:20])[N:5]([CH3:21])[C:4]=2[N:3]=1.[NH:22]1[CH2:28][CH2:27][CH2:26][CH2:25][CH:24]([NH2:29])[CH2:23]1.C(N(CC)CC)C.O>CS(C)=O.ClCCl>[NH2:29][CH:24]1[CH2:25][CH2:26][CH2:27][CH2:28][N:22]([C:2]2[N:10]([CH2:11][C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[Br:18])[C:9]3[C:8](=[O:19])[NH:7][C:6](=[O:20])[N:5]([CH3:21])[C:4]=3[N:3]=2)[CH2:23]1

참가 물질

7

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 2756445Azepan-3-amineHCID 225085758-Bromo-7-(2-bromobenzyl)-3-methyl-3,7-dihydropurine-2,6-dione

생성물 1

HCID 225086388-(3-Aminoazepan-1-yl)-7-(2-bromobenzyl)-3-methyl-3,7-dihydropurine-2,6-dione

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 6344Dichloromethane용매

실험 절차

8-Bromo-7-(2-bromobenzyl)-3-methyl-3,7-dihydropurine-2,6-dione (80A) (300 mg, 0,7 mmol) and azepan-3-ylamine (248 mg, 2,2 mmol), and triethylamine (0.5 ml, 3,6 mmol) were dissolved in 3 ml of DMSO and the mixture was subjected to microwaves (method F, 200° C., 300 W) for 30 minutes. To the reaction mixture was added 100 ml of water and 100 ml of dichloromethane, and the organic layer was separated and dried over sodium sulfate. The solvents were evaporated and the crude product was purified by preparative HPLC (method A1, Rt=7.17 min.). Evaporation of the solvent afforded the title compound as an brown oil.

후처리

  1. customthe organic layer was separated
  2. dry with materialdried over sodium sulfate
  3. customThe solvents were evaporated
  4. customthe crude product was purified by preparative HPLC (method A1, Rt=7.17 min.)
  5. customEvaporation of the solvent

출처 및 근거

ORD 기록
ord-f63a5f954fff49b69eb65b75e3ab1433
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07192952B2

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