Water → HCID 22508608, 화합물

HRID 984829노트

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HRID 984829 반응식
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

참가 물질

7

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 2756445Azepan-3-amineHCID 22508571HCID 22508571, 화합물

생성물 1

HCID 22508608HCID 22508608, 화합물

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 6344Dichloromethane용매

실험 절차

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.

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=8.77 min.)
  5. customEvaporation of the solvent

출처 및 근거

ORD 기록
ord-f4625e3b97d54440990f05fef183ae97
출처 데이터셋
uspto-grants-2005_03
특허 번호
US06869947B2

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