Nitrogen → HCID 42643916、化合物

HRID 42942ノート

反応式

HRID 42942 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]=[CH:22][O:23][C:24]=3[C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][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]=[CH:22][O:23][C:24]=3[C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=3)=[O:19])[CH:14]=[N:13]2)=[CH:9][N:10]=1)(=[O:3])[CH3:5]

参加物

5

反応物 2

HCID 947NitrogenHCID 673662405-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 42643916HCID 42643916、化合物

試薬・触媒・溶媒 2

HCID 14801Manganese dioxide触媒HCID 694302-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 5-phenyl-oxazole-4-carboxylic acid {2-[2-(1-hydroxy-ethyl)-oxazol-5-ylmethyl]-2H-[1,2,3]triazol-4-yl}-amide (60 mg, 0.16 mmol) in AcCN (1.6 mL) was treated at rt with MnO2 (114 mg, 1.18 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 foam. LC-MS-conditions 02: tR=0.97 min; [M+H]+=379.06.

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-4d2287d3714346128aa814709186d15d
出典データセット
uspto-grants-2013_09
特許番号
US08536209B2

反応ノート

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