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Nitrogen → 2-Methyl-5-(3-trifluoromethoxy-phenyl)-oxazole-4-carboxylic acid [2-(2-acetyl-oxazol-5-ylmethyl)-2H-[1,2,3]triazol-4-yl]-amide

HRID 42974
ノート
印刷プレビュー

反応式

HRID 42974 の反応式
N#N.[OH:3][CH:4]([C:6]1[O:7][C:8]([CH2:11][N:12]2[N:16]=[C:15]([NH:17][C:18]([C:20]3[N:21]=[C:22]([CH3:36])[O:23][C:24]=3[C:25]3[CH:30]=[CH:29][CH:28]=[C:27]([O:31][C:32]([F:35])([F:34])[F:33])[CH:26]=3)=[O:19])[CH:14]=[N:13]2)=[CH:9][N:10]=1)[CH3:5]>C(C#N)(C)=O.O=[Mn]=O>[C:4]([C:6]1[O:7][C:8]([CH2:11][N:12]2[N:16]=[C:15]([NH:17][C:18]([C:20]3[N:21]=[C:22]([CH3:36])[O:23][C:24]=3[C:25]3[CH:30]=[CH:29][CH:28]=[C:27]([O:31][C:32]([F:34])([F:35])[F:33])[CH:26]=3)=[O:19])[CH:14]=[N:13]2)=[CH:9][N:10]=1)(=[O:3])[CH3:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 947NitrogenHCID 673650542-Methyl-5-(3-trifluoromethoxy-phenyl)-oxazole-4-carboxylic acid {2-[2-(1-hydroxy-ethyl)-oxazol-5-ylmethyl]-2H-[1,2,3]triazol-4-yl}-amide

生成物 1

HCID 673652652-Methyl-5-(3-trifluoromethoxy-phenyl)-oxazole-4-carboxylic acid [2-(2-acetyl-oxazol-5-ylmethyl)-2H-[1,2,3]triazol-4-yl]-amide

試薬・触媒・溶媒 2

HCID 14801Manganese dioxide触媒
HCID 69430
2-Oxopropiononitrile
溶媒

実験手順

In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a solution of 2-methyl-5-(3-trifluoromethoxy-phenyl)-oxazole-4-carboxylic acid {2-[2-(1-hydroxy-ethyl)-oxazol-5-ylmethyl}-2H-[1,2,3]triazol-4-yl]-amide (54 mg, 0.11 mmol) in AcCN (1.5 mL) was treated at rt with MnO2 (85 mg, 0.85 mmol) and the reaction mixture was stirred at rt overnight before being filtered through Celite. The solvent was removed under reduced pressure and the residue was dissolved in EA (10 mL), washed with water (10 mL), and brine. The org. layer was dried over MgSO4, filtered, and the solvents were removed under reduced pressure to give the title compound as a white solid. LC-MS-conditions 02: tR=1.09 min; [M+H]+=476.95.

後処理

  1. filtrationbefore being filtered through Celite
  2. customThe solvent was removed under reduced pressure
  3. dissolutionthe residue was dissolved in EA (10 mL)
  4. washwashed with water (10 mL), and brine
  5. dry with materiallayer was dried over MgSO4
  6. filtrationfiltered
  7. customthe solvents were removed under reduced pressure

出典と根拠

ORDレコード
ord-3cc3e3f5229e4e038ed82bffc1339204
出典データセット
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08536209B2

反応ノート

読み込み中…

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