Water → HCID 22508608、化合物

HRID 984829ノート

反応式

HRID 984829 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[Cl:18])[C:9]2[C:8](=[O:19])[N:7]([CH2:20][C:21]3[CH:28]=[CH:27][CH:26]=[CH:25][C:22]=3[C:23]#[N:24])[C:6](=[O:29])[N:5]([CH3:30])[C:4]=2[N:3]=1.[NH:31]1[CH2:37][CH2:36][CH2:35][CH2:34][CH:33]([NH2:38])[CH2:32]1.C(N(CC)CC)C.O>CS(C)=O.ClCCl>[NH2:38][CH:33]1[CH2:34][CH2:35][CH2:36][CH2:37][N:31]([C:2]2[N:10]([CH2:11][C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[Cl:18])[C:9]3[C:8](=[O:19])[N:7]([CH2:20][C:21]4[CH:28]=[CH:27][CH:26]=[CH:25][C:22]=4[C:23]#[N:24])[C:6](=[O:29])[N:5]([CH3:30])[C:4]=3[N:3]=2)[CH2:32]1

参加物

7

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 2756445Azepan-3-amineHCID 22508571HCID 22508571、化合物

生成物 1

HCID 22508608HCID 22508608、化合物

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 6344Dichloromethane溶媒

実験手順

2-(8-Bromo-7-(2-chlorobenzyl)-3-methyl-2,6-dioxo-1,2,3,6-tetrahydropurin-1-ylmethyl)benzonitrile (75B) (250 mg, 0.5 mmol) and azepan-3-ylamine (294 mg, 2.5 mmol), and triethylamine (0.35 ml, 2.5 mmol) were dissolved in 20 ml of DMSO and the mixture was subjected to microwaves (method F, 100° C., 300 W) for five hours. 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=8.77 min.). Evaporation of the solvent afforded the title compound as an yellow 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=8.77 min.)
  5. customEvaporation of the solvent

出典と根拠

ORDレコード
ord-f4625e3b97d54440990f05fef183ae97
出典データセット
uspto-grants-2005_03
特許番号
US06869947B2

反応ノート

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