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

HRID 458639ノート

反応式

HRID 458639 の反応式
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

参加物

7

反応物 5

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5cbfa1b9329d467789a6ecafe5ce2d14
出典データセット
uspto-grants-2007_03
特許番号
US07192952B2

反応ノート

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