Dimethyl Sulfoxide → 8-(3-Aminoazepan-1-yl)-3-methyl-7-(2-trifluoromethylbenzyl)-3,7-dihydropurine-2,6-dione TFA

HRID 458639노트

반응식

HRID 458639 반응식
Br[C:2]1[N:10]([CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=2[C:18]([F:21])([F:20])[F:19])[C:9]2[C:8](=[O:22])[NH:7][C:6](=[O:23])[N:5]([CH3:24])[C:4]=2[N:3]=1.[NH:25]1[CH2:31][CH2:30][CH2:29][CH2:28][CH:27]([NH2:32])[CH2:26]1.C(N(CC)CC)C.[OH2:40].CS(C)=[O:43]>ClCCl>[OH:40][C:13]([C:18]([F:21])([F:20])[F:19])=[O:43].[NH2:32][CH:27]1[CH2:28][CH2:29][CH2:30][CH2:31][N:25]([C:2]2[N:10]([CH2:11][C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[C:18]([F:21])([F:19])[F:20])[C:9]3[C:8](=[O:22])[NH:7][C:6](=[O:23])[N:5]([CH3:24])[C:4]=3[N:3]=2)[CH2:26]1

참가 물질

7

반응물 5

HCID 679Dimethyl SulfoxideHCID 962WaterHCID 8471TriethylamineHCID 2756445Azepan-3-amineHCID 225086498-Bromo-3-methyl-7-(2-trifluoromethylbenzyl)-3,7-dihydropurine-2,6-dione

생성물 1

HCID 1317247998-(3-Aminoazepan-1-yl)-3-methyl-7-(2-trifluoromethylbenzyl)-3,7-dihydropurine-2,6-dione TFA

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

8-Bromo-3-methyl-7-(2-trifluoromethylbenzyl)-3,7-dihydropurine-2,6-dione (81A) (300 mg, 0.7 mmol) and azepan-3-ylamine (255 mg, 2,2 mmol), and triethylamine (0.5 ml, 3.7 mmol) were dissolved in 3 ml of DMSO and the mixture was subjected to microwaves (method F, 200° C., 300 W) for 10 minutes. To the reaction mixture was added 100 ml of water and 100 ml of dichloromethane, and the organic layer was washed with 1N NaOH, and dried over sodium sulfate. The solvents were evaporated and the crude product was purified by preparative HPLC (method A1, Rt=7.42 min.). Evaporation of the solvent afforded the title compound as a brown oil.

후처리

  1. washthe organic layer was washed with 1N NaOH
  2. dry with materialdried over sodium sulfate
  3. customThe solvents were evaporated
  4. customthe crude product was purified by preparative HPLC (method A1, Rt=7.42 min.)
  5. customEvaporation of the solvent

출처 및 근거

ORD 기록
ord-5cbfa1b9329d467789a6ecafe5ce2d14
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07192952B2

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