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Potassium Carbonate → HCID 86677483、化合物

HRID 1621126
ノート
印刷プレビュー

反応式

HRID 1621126 の反応式
[CH3:1][C:2]1[NH:6][N:5]=[C:4]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[N:3]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:20][CH2:21][NH:22][C:23](=[O:29])[O:24][C:25]([CH3:28])([CH3:27])[CH3:26]>CN(C=O)C>[CH3:1][C:2]1[N:6]([CH2:20][CH2:21][NH:22][C:23](=[O:29])[O:24][C:25]([CH3:28])([CH3:27])[CH3:26])[N:5]=[C:4]([C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=2)[N:3]=1
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 3

HCID 11430Potassium CarbonateHCID 5943813-methyl-5-phenyl-1H-1,2,4-triazoleHCID 4103526tert-Butyl N-(2-bromoethyl)carbamate

生成物 1

HCID 86677483HCID 86677483、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

5-Methyl-3-phenyl-1H-1,2,4-triazole (120 mg, 754 μmol) was dissolved in DMF (2.4 mL) and potassium carbonate (208 mg, 1.51 mmol) was added. After 20 min tert-butyl 2-bromoethylcarbamate (186 mg, 829 μmol) was added at 0-5° C. and the reaction mixture was stirred at RT for 25 h. The reaction mixture was extracted with ethyl acetate (30 mL) and washed with water (3×50 mL). The aqueous layers were back-extracted with ethyl acetate (20 mL) and the combined organic layer was dried over MgSO4 and concentrated in vacuo. The product was obtained after purification by flash chromatography (using silica gel and an ethyl acetate/heptane gradient) as white solid (237 mg, 784 μmol, 83.2%).

後処理

  1. extractionThe reaction mixture was extracted with ethyl acetate (30 mL)
  2. washwashed with water (3×50 mL)
  3. extractionThe aqueous layers were back-extracted with ethyl acetate (20 mL)
  4. dry with materialthe combined organic layer was dried over MgSO4
  5. concentrationconcentrated in vacuo
  6. customThe product was obtained
  7. customafter purification by flash chromatography (

出典と根拠

ORDレコード
ord-eb6745774e6842659b87fa0756d1ffb2
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08772510B2

反応ノート

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