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tert-butyl 4-(4-amino-6-(3-(pyrrolidin-1-yl)propyl)pyrrolo[2,1-f][1,2,4]triazin-7-yl)-5,6-dihydropyridine-1(2H)-carboxylate → Tert-butyl 4-(4-amino-6-(3-(pyrrolidin-1-yl)propyl)pyrrolo[2,1-f][1,2,4]triazin-7-yl)piperidine-1-carboxylate

HRID 1615468
ノート
印刷プレビュー

反応式

HRID 1615468 の反応式
[NH2:1][C:2]1[C:7]2=[CH:8][C:9]([CH2:24][CH2:25][CH2:26][N:27]3[CH2:31][CH2:30][CH2:29][CH2:28]3)=[C:10]([C:11]3[CH2:16][CH2:15][N:14]([C:17]([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18])[CH2:13][CH:12]=3)[N:6]2[N:5]=[CH:4][N:3]=1>C([O-])(=O)C.[Pt](=O)=O>[NH2:1][C:2]1[C:7]2=[CH:8][C:9]([CH2:24][CH2:25][CH2:26][N:27]3[CH2:31][CH2:30][CH2:29][CH2:28]3)=[C:10]([CH:11]3[CH2:16][CH2:15][N:14]([C:17]([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18])[CH2:13][CH2:12]3)[N:6]2[N:5]=[CH:4][N:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 66601711tert-butyl 4-(4-amino-6-(3-(pyrrolidin-1-yl)propyl)pyrrolo[2,1-f][1,2,4]triazin-7-yl)-5,6-dihydropyridine-1(2H)-carboxylate

生成物 1

HCID 66614420Tert-butyl 4-(4-amino-6-(3-(pyrrolidin-1-yl)propyl)pyrrolo[2,1-f][1,2,4]triazin-7-yl)piperidine-1-carboxylate収率 100.1%

試薬・触媒・溶媒 2

HCID 345198Adams' catalyst触媒HCID 175Acetate溶媒

実験手順

In a pressure reactor (50 mL), a mixture of the compound (132 mg, 0.31 mmol) prepared in Example 17 and platinum (IV) oxide in acetyl hydroxide (10 mL) was stirred under hydrogen atmosphere (3 atm). At 6 hours, the mixture was filtered through celite, eluting with acetyl hydroxide. The solvent was removed in vacuo. The resulting material extracted with DCM/sodium bicarbonate aqueous solution. The organic layers were dried over sodium sulfate, filtered and the solvent removed in vacuum to obtain the title compound (133 mg) having the following physical data.

後処理

  1. filtrationthe mixture was filtered through celite
  2. washeluting with acetyl hydroxide
  3. customThe solvent was removed in vacuo
  4. extractionThe resulting material extracted with DCM/sodium bicarbonate aqueous solution
  5. dry with materialThe organic layers were dried over sodium sulfate
  6. filtrationfiltered
  7. customthe solvent removed in vacuum

出典と根拠

ORDレコード
ord-0e9a2bccad184a8e878e419f8f6f8ad1
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08765754B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート