Sulfuric Acid → HCID 69735154、化合物

HRID 1814613ノート

反応式

HRID 1814613 の反応式
[Br:1][C:2]1[CH:15]=[CH:14][C:5]([C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=O)=[CH:4][CH:3]=1.C(OP([CH2:24][C:25]1[CH:30]=[C:29]([O:31][CH2:32][CH3:33])[C:28]([CH2:34]P(OCC)(OCC)=O)=[CH:27][C:26]=1[O:43][CH2:44][CH3:45])(OCC)=O)C.[C:46](O[K])([CH3:49])([CH3:48])[CH3:47].S(=O)(=O)(O)O>O1CCCC1.O>[Br:1][C:2]1[CH:15]=[CH:14][C:5]([C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[CH:34][C:28]2[CH:27]=[C:26]([O:43][CH2:44][CH3:45])[C:25]([CH:24]=[C:47]([C:8]3[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=3)[C:46]3[CH:49]=[CH:15][C:2]([Br:1])=[CH:3][CH:48]=3)=[CH:30][C:29]=2[O:31][CH2:32][CH3:33])=[CH:4][CH:3]=1

参加物

7

反応物 4

HCID 1118Sulfuric AcidHCID 70304-BromobenzophenoneHCID 2785335HCID 2785335、化合物HCID 178418922HCID 178418922、化合物

生成物 1

HCID 69735154HCID 69735154、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒2 回

実験手順

Under an inert atmosphere, 4-bromobenzophenone (2.611 g, 10 mmol), and 1,4-bis(diethylphosphonomethyl)-2,5-diethoxybenzene (1.912 g, 4.10 mmol) are dissolved in tetrahydrofuran (30 g). At room temperature, tetrahydrofuran (10.92 g) solution of tert-butoxy potassium (1.380 g, 12.30 mmol) is added dropwise for 5 minutes, and successively stirred for 3.5 hours. The reaction mixture is charged into water (200 ml) and neutralized with 5% sulfuric acid. After neutralization, a hydrophobic solvent is added and the organic layer is partitioned. The organic layer is washed with water and dried over anhydrous sodium sulfate. The solvent is distilled off under reduced pressure, and the resultant raw product is purified by silica gel chromatography or recrystallization to give a desired product.

後処理

  1. additionAfter neutralization, a hydrophobic solvent is added
  2. customthe organic layer is partitioned
  3. washThe organic layer is washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationThe solvent is distilled off under reduced pressure
  6. customthe resultant raw product is purified by silica gel chromatography or recrystallization

出典と根拠

ORDレコード
ord-95652d3e3c27438cb5239e863db58d97
出典データセット
uspto-grants-2005_04
特許番号
US06875895B2

反応ノート

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