Sodium Hydroxide → HCID 90403762、化合物

HRID 2200616ノート

反応式

HRID 2200616 の反応式
[NH2:1][C:2]1[N:7]([CH3:8])[C:6](=[O:9])[N:5]([CH2:10][C:11]2[CH:16]=[CH:15][C:14]([O:17][CH3:18])=[CH:13][CH:12]=2)[C:4](=[O:19])[C:3]=1[NH:20][C:21](=O)[CH2:22][CH2:23][CH2:24][O:25][C:26]1[CH:31]=[CH:30][CH:29]=[C:28]([O:32][C:33]([F:36])([F:35])[F:34])[CH:27]=1.[OH-].[Na+].[Cl-].[NH4+]>C(O)C>[CH3:18][O:17][C:14]1[CH:15]=[CH:16][C:11]([CH2:10][N:5]2[C:4](=[O:19])[C:3]3[NH:20][C:21]([CH2:22][CH2:23][CH2:24][O:25][C:26]4[CH:31]=[CH:30][CH:29]=[C:28]([O:32][C:33]([F:36])([F:35])[F:34])[CH:27]=4)=[N:1][C:2]=3[N:7]([CH3:8])[C:6]2=[O:9])=[CH:12][CH:13]=1

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 25517Ammonium ChlorideHCID 90402822HCID 90402822、化合物

生成物 1

HCID 90403762HCID 90403762、化合物収率 89.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
80 °C

実験手順

To a solution of N-(6-amino-3-(4-methoxybenzyl)-1-methyl-2,4-dioxo-1,2,3,4-tetrahydropyrimidin-5-yl)-4-(3-(trifluoromethoxy)phenoxy)butanamide (150 mg, 0.287 mmol) in ethanol (7 mL) was added 2N NaOH (1 mL). The mixture was stirred at 80° C. for 3 h. The reaction was neutralized with saturated ammonium chloride and the product precipitated. The solids were collected and washed with water. The solids were dissolved in ethyl acetate, dried over sodium sulfate and concentrated to give 1-(4-methoxybenzyl)-3-methyl-8-(3-(3-(trifluoromethoxy)phenoxy)propyl)-1H-purine-2,6(3H,7H)-dione (130 mg, 89.7%) as a light yellow solid. LCMS retention time 1.635 min; LCMS MH+ 505.

後処理

  1. customthe product precipitated
  2. customThe solids were collected
  3. washwashed with water
  4. dissolutionThe solids were dissolved in ethyl acetate
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-ba65e9835b344e29a55d4d57b5660fa2
出典データセット
uspto-grants-2016_06
特許番号
US09359359B2

反応ノート

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