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Sulfuric Acid → HCID 69735150、化合物

HRID 1814608
ノート
印刷プレビュー

反応式

HRID 1814608 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][CH3:32])[C:28]([CH2:33]P(OCC)(OCC)=O)=[CH:27][C:26]=1[O:42][CH2:43][CH:44]([CH2:49][CH3:50])[CH2:45][CH2:46][CH2:47][CH3:48])(OCC)=O)C.[C:51](O[K])([CH3:54])([CH3:53])[CH3:52].S(=O)(=O)(O)O>O1CCCC1.C(OCC)(=O)C.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:24][C:25]2[CH:30]=[C:29]([O:31][CH3:32])[C:28]([CH:33]=[C:52]([C:8]3[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=3)[C:51]3[CH:54]=[CH:15][C:2]([Br:1])=[CH:3][CH:53]=3)=[CH:27][C:26]=2[O:42][CH2:43][CH:44]([CH2:49][CH3:50])[CH2:45][CH2:46][CH2:47][CH3:48])=[CH:4][CH: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

8

反応物 4

HCID 1118Sulfuric AcidHCID 70304-BromobenzophenoneHCID 58887345HCID 58887345、化合物HCID 178418922HCID 178418922、化合物

生成物 1

HCID 69735150HCID 69735150、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒
HCID 8028
Tetrahydrofuran
溶媒
2 回
HCID 8857Ethyl Acetate溶媒

実験手順

Under an inert atmosphere, 4-bromobenzophenone (0.783 g, 3mmol), and 1,4-bis-(diethylphosphonomethyl)-2-(2-ethylhexyloxy)-5-methoxy benzene (0.660 g, 1.23 mmol) were dissolved in tetrahydrofuran (10 g). At room temperature, tetrahydrofuran (3.28 g) solution of tert-butoxy potassium (0.414 g, 3.69 mmol) was added dropwise for 5 minutes, and successively stirred for 3.5 hours. The reaction mixture was charged into water (100 ml) and neutralized with 5% sulfuric acid. After neutralization, ethyl acetate (250 ml) was added and the organic layer was partitioned. The organic layer was washed with water and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, and the resultant raw product was purified by silica gel chromatography to give the desired product. (Yield: 0.86 g, 93%)

後処理

  1. customthe organic layer was partitioned
  2. washThe organic layer was washed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationThe solvent was distilled off under reduced pressure
  5. customthe resultant raw product was purified by silica gel chromatography

出典と根拠

ORDレコード
ord-f1ad3f57de03421082d4a0d31ddd2a74
出典データセット
uspto-grants-2005_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06875895B2

反応ノート

読み込み中…

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