Potassium Carbonate → HCID 90402978、化合物

HRID 2200600ノート

反応式

HRID 2200600 の反応式
[CH3:1][O:2][C:3]1[CH:33]=[CH:32][C:6]([CH2:7][N:8]2[C:16](=[O:17])[C:15]3[NH:14][C:13]([CH2:18][C:19]4[CH:24]=[CH:23][CH:22]=[C:21]([O:25][C:26]([F:29])([F:28])[F:27])[CH:20]=4)=[N:12][C:11]=3[N:10]([CH3:30])[C:9]2=[O:31])=[CH:5][CH:4]=1.Cl[CH2:35][C:36]1[CH:41]=[CH:40][C:39]([CH3:42])=[CH:38][N:37]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([CH2:7][N:8]2[C:16](=[O:17])[C:15]3[N:14]([CH2:35][C:36]4[CH:41]=[CH:40][C:39]([CH3:42])=[CH:38][N:37]=4)[C:13]([CH2:18][C:19]4[CH:24]=[CH:23][CH:22]=[C:21]([O:25][C:26]([F:27])([F:29])[F:28])[CH:20]=4)=[N:12][C:11]=3[N:10]([CH3:30])[C:9]2=[O:31])=[CH:32][CH:33]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 5880562-(Chloromethyl)-5-methylpyridine2 回HCID 90402923HCID 90402923、化合物2 回

生成物 1

HCID 90402978HCID 90402978、化合物収率 89.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
55 °C

実験手順

To a solution of 1-(4-methoxybenzyl)-3-methyl-8-(3-(trifluoromethoxy)benzyl)-1H-purine-2,6(3H,7H)— dione (110 mg, 0.238 mmol, intermediate 48) in DMF (4 mL) was added 2-(chloromethyl)-5-methylpyridine (33.8 mg, 0.238 mmol, intermediate 50), followed by potassium carbonate (49.5 mg, 0.358 mmol). The reaction was stirred at 55° C. for 2 h. The mixture was partitioned between ethyl acetate and water. The organic phase was washed with brine, dried over sodium sulfate, filtered and concentrated to give a white solid product (120 mg, 88.8% yield) which was used without purification. LCMS MH+ 566.

後処理

  1. customThe mixture was partitioned between ethyl acetate and water
  2. washThe organic phase was washed with brine
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-7aa780a0174c41b4aea657b2b0ae3f62
出典データセット
uspto-grants-2016_06
特許番号
US09359359B2

反応ノート

読み込み中…