Nitrogen → HCID 67364278、化合物

HRID 42807ノート

反応式

HRID 42807 の反応式
N#N.[CH3:3][C:4]1([C:9]2[CH:14]=[C:13]([CH2:15][N:16]3[N:20]=[C:19]([N+:21]([O-])=O)[CH:18]=[N:17]3)[CH:12]=[CH:11][N:10]=2)[O:8][CH2:7][CH2:6][O:5]1.[NH4+].[Cl-]>CCO.O.[Fe]>[CH3:3][C:4]1([C:9]2[CH:14]=[C:13]([CH2:15][N:16]3[N:20]=[C:19]([NH2:21])[CH:18]=[N:17]3)[CH:12]=[CH:11][N:10]=2)[O:8][CH2:7][CH2:6][O:5]1

参加物

7

反応物 3

HCID 947NitrogenHCID 25517Ammonium ChlorideHCID 673655522-(2-Methyl-[1,3]dioxolan-2-yl)-4-(4-nitro-[1,2,3]triazol-2-ylmethyl)-pyridine

生成物 1

HCID 67364278HCID 67364278、化合物

試薬・触媒・溶媒 3

HCID 23925Iron触媒HCID 702Ethanol溶媒HCID 962Water溶媒

反応条件

温度
75 °C

実験手順

In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a mixture of 2-(2-methyl-[1,3]dioxolan-2-yl)-4-(4-nitro-[1,2,3]triazol-2-ylmethyl)-pyridine (145 mg, 0.50 mmol), iron powder (84 mg, 1.49 mmol) and NH4Cl (134 mg, 2.49 mmol) in a mixture of EtOH (2.0 mL) and water (1.0 mL) was stirred at 75° C. for 60 min. The reaction mixture was filtered while hot and concentrated under reduced pressure. CH2Cl2 (10 mL) was added followed by 1N NaOH (10 mL). The aq. layer was extracted with CH2Cl2 (2×10 mL) and the combined org. extracts were dried over MgSO4, filtered, and the solvents were removed under reduced pressure to give the title compound as a light yellow oil. LC-MS-conditions 02: tR=0.54 min; [M+H]+=261.78.

後処理

  1. filtrationThe reaction mixture was filtered while hot and
  2. concentrationconcentrated under reduced pressure
  3. additionCH2Cl2 (10 mL) was added
  4. extractionThe aq. layer was extracted with CH2Cl2 (2×10 mL)
  5. dry with materialextracts were dried over MgSO4
  6. filtrationfiltered
  7. customthe solvents were removed under reduced pressure

出典と根拠

ORDレコード
ord-93af6668341f4e349fc9a58b211f9954
出典データセット
uspto-grants-2013_09
特許番号
US08536209B2

反応ノート

読み込み中…