Sulfuric Acid → HCID 69735154, 화합물

HRID 1814613노트

반응식

HRID 1814613 반응식
[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

참가 물질

7

반응물 4

HCID 1118Sulfuric AcidHCID 70304-BromobenzophenoneHCID 2785335HCID 2785335, 화합물HCID 178418922HCID 178418922, 화합물

생성물 1

HCID 69735154HCID 69735154, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-95652d3e3c27438cb5239e863db58d97
출처 데이터셋
uspto-grants-2005_04
특허 번호
US06875895B2

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