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m-Chloroperbenzoic acid → N-(4-tert-Butylphenyl)-7-(3-chloropyridin-2-yl)-5,6,7,8-tetrahydro-2-methoxypyrido[3,4-d]pyrimidin-4-amine

HRID 2219961
ノート
印刷プレビュー

反応式

HRID 2219961 の反応式
C1C=C(Cl)C=C([C:8](OO)=[O:9])C=1.[C:12]([C:16]1[CH:21]=[CH:20][C:19]([NH:22][C:23]2[C:24]3[CH2:34][CH2:33][N:32]([C:35]4[C:40]([Cl:41])=[CH:39][CH:38]=[CH:37][N:36]=4)[CH2:31][C:25]=3[N:26]=[C:27](SC)[N:28]=2)=[CH:18][CH:17]=1)([CH3:15])([CH3:14])[CH3:13].C[O-].[Na+]>C(O)C>[C:12]([C:16]1[CH:21]=[CH:20][C:19]([NH:22][C:23]2[C:24]3[CH2:34][CH2:33][N:32]([C:35]4[C:40]([Cl:41])=[CH:39][CH:38]=[CH:37][N:36]=4)[CH2:31][C:25]=3[N:26]=[C:27]([O:9][CH3:8])[N:28]=2)=[CH:18][CH:17]=1)([CH3:15])([CH3:14])[CH3:13]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 70297m-Chloroperbenzoic acidHCID 10942334Sodium MethoxideHCID 12004390N-(4-tert-Butylphenyl)-7-(3-chloropyridin-2-yl)-5,6,7,8-tetrahydro-2-(methylthio)pyrido[3,4-d]pyrimidin-4-amine

生成物 1

HCID 12004391N-(4-tert-Butylphenyl)-7-(3-chloropyridin-2-yl)-5,6,7,8-tetrahydro-2-methoxypyrido[3,4-d]pyrimidin-4-amine収率 39%

試薬・触媒・溶媒 1

HCID 702
Ethanol
溶媒

反応条件

温度
60 °C

実験手順

m-CPBA (148 mg, 0.6 mmol) was added to the solution of N-(4-tert-butylphenyl)-7-(3-chloropyridin-2-yl)-5,6,7,8-tetrahydro-2-(methylthio)pyrido[3,4-d]pyrimidin-4-amine from Example 28.C. (88 mg, 0.2 mmol) in ethanol (7 mL) and stirred at room temperature for 1 hr. Solid thus formed was filtered out and dried in vacuo (50 mg). This solid was suspended in methanol (5 mL) and sodium methoxide (9 mg, 0.165 mmol) was added and stirred at 60° C. overnight. Solvent was removed in vacuo and residue was dissolved in ethyl acetate, washed by water, sodium hydrosulfite aqueous solution, brine and dried over sodium sulfate. Purified by column to yield the product as a white solid (33 mg, 39%).

後処理

  1. customSolid thus formed
  2. filtrationwas filtered out
  3. customdried in vacuo (50 mg)
  4. customSolvent was removed in vacuo and residue
  5. dissolutionwas dissolved in ethyl acetate
  6. washwashed by water, sodium hydrosulfite aqueous solution, brine
  7. dry with materialdried over sodium sulfate
  8. customPurified by column

出典と根拠

ORDレコード
ord-821080b30b3049759a34dae54ae14429
出典データセット
uspto-grants-2008_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07414131B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート