Potassium Carbonate → HCID 58276234、化合物

HRID 471826

反応式

HRID 471826 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([C:8]2[N:12]=[CH:11][NH:10][N:9]=2)[CH:5]=[CH:6][CH:7]=1.[C:13]([O-])([O-])=O.[K+].[K+].ClC[CH2:21][C:22]([CH3:27])([CH3:26])[C:23]([O-:25])=[O:24]>CC#N>[CH3:21][C:22]([CH3:27])([CH3:26])[C:23]([O:25][CH2:13][N:10]1[CH:11]=[N:12][C:8]([C:4]2[CH:5]=[CH:6][CH:7]=[C:2]([Br:1])[CH:3]=2)=[N:9]1)=[O:24]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 124615465-(3-Bromophenyl)-1H-1,2,4-triazoleHCID 217530474-Chloro-2,2-dimethylbutanoate

生成物 1

HCID 58276234HCID 58276234、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A slurry of 3-(3-bromophenyl)-1H-1,2,4-triazole (58.5 g; 261 mmol; Step 1 above), anhydrous K2CO3 (43.2 g; 313 mmol), and chloromethylpivalate (45 mL; 313 mmol) in dry MeCN (250 mL) was heated to 80° C. (Note 1) for 1 hour. The mixture was cooled, solid was collected by filtration and the filtrate was concentrated in vacuo. Residue from the filtaret was combined with the filtered solid and the whole was stirred with water approximately 20 minutes. Solid was collected by filtration, washed with water (×3) and recrystallized from MeOH/water, affording the title compound as a colorless solid. LC/MS (method E) tR 0.88 min, m/z 338, 340 (M+H, Br isotopes).

後処理

  1. temperatureThe mixture was cooled
  2. filtrationsolid was collected by filtration
  3. concentrationthe filtrate was concentrated in vacuo
  4. filtrationSolid was collected by filtration
  5. washwashed with water (×3)
  6. customrecrystallized from MeOH/water

出典と根拠

ORDレコード
ord-a20f4023092e43399ab9bce74f429690
出典データセット
uspto-grants-2014_01
特許番号
US08633175B2

関連ノート

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