Tetrabutylammonium Fluoride → 5-(1-Methyl-1H-1,2,3-triazol-4-yl)-2-{[6-(morpholin-4-ylmethyl)pyridin-2-yl]amino}thiophene-3-carboxamide

HRID 386145

反応式

HRID 386145 の反応式
[N:1]1([CH2:7][C:8]2[N:13]=[C:12]([NH:14][C:15]3[S:16][C:17]([C:23]4[N:24]=[N:25][N:26]([CH2:28][Si](C)(C)C)[CH:27]=4)=[CH:18][C:19]=3[C:20]([NH2:22])=[O:21])[CH:11]=[CH:10][CH:9]=2)[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.CCCC[N+](CCCC)(CCCC)CCCC.[F-]>C1COCC1.O>[CH3:28][N:26]1[CH:27]=[C:23]([C:17]2[S:16][C:15]([NH:14][C:12]3[CH:11]=[CH:10][CH:9]=[C:8]([CH2:7][N:1]4[CH2:2][CH2:3][O:4][CH2:5][CH2:6]4)[N:13]=3)=[C:19]([C:20]([NH2:22])=[O:21])[CH:18]=2)[N:24]=[N:25]1

参加物

5

反応物 2

HCID 2724141Tetrabutylammonium FluorideHCID 595255682-{[6-(Morpholin-4-ylmethyl)pyridin-2-yl]amino}-5-{1-[(trimethylsilyl)methyl]-1H-1,2,3-triazol-4-yl}thiophene-3-carboxamide

生成物 1

HCID 595257025-(1-Methyl-1H-1,2,3-triazol-4-yl)-2-{[6-(morpholin-4-ylmethyl)pyridin-2-yl]amino}thiophene-3-carboxamide

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 2-{[6-(morpholin-4-ylmethyl)pyridin-2-yl]amino}-5-{1-[(trimethylsilyl)methyl]-1H-1,2,3-triazol-4-yl}thiophene-3-carboxamide (65 mg, 0.14 mmol) in THF (2.0 mL) was added TBAF (1.0 M in THF, 0.276 ml, 0.276 mmol). The reaction was stirred at room temperature for 4 h. The solution was diluted with water and extracted with 5:1 CH2Cl2:MeOH (3×). The combined organic layers were dried (MgSO4), filtered, and evaporated. The crude solid was triturated with CH2Cl2 and filtered to isolate the title compound as a colorless solid.

後処理

  1. extractionextracted with 5:1 CH2Cl2
  2. dry with materialThe combined organic layers were dried (MgSO4)
  3. filtrationfiltered
  4. customevaporated
  5. customThe crude solid was triturated with CH2Cl2
  6. filtrationfiltered

出典と根拠

ORDレコード
ord-b5cec79b66c3402f93cfa6f31eec522e
出典データセット
uspto-grants-2013_02
特許番号
US08367706B2

関連ノート

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