Isopropanol → HCID 86619830、化合物

HRID 658337ノート

反応式

HRID 658337 の反応式
[C:1]([O:5][C:6]1[CH:11]=[C:10]([N:12]=[C:13]=[S:14])[CH:9]=[C:8]([F:15])[CH:7]=1)([CH3:4])([CH3:3])[CH3:2].C(N(CC)CC)C.[CH:23]([OH:26])([CH3:25])[CH3:24]>>[CH:23]([O:26][C:13](=[S:14])[NH:12][C:10]1[CH:9]=[C:8]([F:15])[CH:7]=[C:6]([O:5][C:1]([CH3:4])([CH3:2])[CH3:3])[CH:11]=1)([CH3:25])[CH3:24]

参加物

4

反応物 3

HCID 3776IsopropanolHCID 8471TriethylamineHCID 86619831HCID 86619831、化合物

生成物 1

HCID 86619830HCID 86619830、化合物

反応条件

温度
0 °C

実験手順

1-tert-Butoxy-3-fluoro-5-isothiocyanato-benzene (24.0 g) and triethylamine (10.9 g) are dissolved in iso-propanol (150 ml). The reaction mixture is refluxed for 18 hours and the solvent is removed by vacuo. The crude product is dissolved in hexane:diethyl ether (19:1). The diethyl ether is removed by vacuo and the solution is cooled to 0° C. for 3 hours. The solution is filtered to give the title compound. 1H nmr (CDCl3, 400 MHz); 8.10 (br s, 1H), 6.65 (br s, 2H), 6.45 (ddd, 1H) 5.60 (sept, 1H), 1.35 (d, 6H), 1.30 (s, 9H).

後処理

  1. temperatureThe reaction mixture is refluxed for 18 hours
  2. customthe solvent is removed by vacuo
  3. dissolutionThe crude product is dissolved in hexane:diethyl ether (19:1)
  4. customThe diethyl ether is removed by vacuo
  5. filtrationThe solution is filtered

出典と根拠

ORDレコード
ord-8d46e93ce18d447ba15bcc64409de4aa
出典データセット
uspto-grants-2011_12
特許番号
US08076489B2

反応ノート

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