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

HRID 458637

反応式

HRID 458637 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[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

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f63a5f954fff49b69eb65b75e3ab1433
出典データセット
uspto-grants-2007_03
特許番号
US07192952B2

関連ノート

読み込み中…