Sulfuric Acid → HCID 178527055、化合物

HRID 490925

反応式

HRID 490925 の反応式
O.[PH2:2]([O-:4])=[O:3].[Na+].[C:6]1([CH2:12][CH2:13][CH:14]=[CH2:15])[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.N(C(C)(C)C#N)=NC(C)(C)C#N.S(=O)(=O)(O)O.C12(N)CC3CC(CC(C3)C1)C2>C(O)C>[C:6]1([CH2:12][CH2:13][CH2:14][CH2:15][PH:2](=[O:4])[OH:3])[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1

参加物

7

反応物 5

HCID 1118Sulfuric AcidHCID 2130AmantadineHCID 6547AzobisisobutyronitrileHCID 130333-ButenylbenzeneHCID 178418950HCID 178418950、化合物

生成物 1

HCID 178527055HCID 178527055、化合物収率 54.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of sodium hypophosphite hydrate (17.6 g, 200 mmol), 4-phenyl-1-butene (10 mL, 66.6 mmol), 2,2′-azobisisobutyronitrile (AlBN) (1 g), conc. sulfuric acid (1 mL) in 200 mL of absolute ethanol was heated to reflux for 17 hours. The reaction mixture was concentrated to an oil, suspended in 70 mL of water, made basic with 50% NaOH and washed with 2×70 mL ether. The aqueous layer was acidified with conc. sulfuric acid, extracted into ethyl acetate and concentrated. The residue was dissolved in ether and adamantaneamine (10 g, 66 mmol) was added. A white precipitate was filtered, partitioned between 10% HCl and ethyl acetate. The organic layer was concentrated to provide 4-phenylbutylphosphinic acid (7.2 g).

後処理

  1. temperatureto reflux for 17 hours
  2. concentrationThe reaction mixture was concentrated to an oil
  3. washwashed with 2×70 mL ether
  4. extractionextracted into ethyl acetate
  5. concentrationconcentrated
  6. dissolutionThe residue was dissolved in ether
  7. filtrationA white precipitate was filtered
  8. custompartitioned between 10% HCl and ethyl acetate
  9. concentrationThe organic layer was concentrated

出典と根拠

ORDレコード
ord-52c6bf5ce5e24e2cb1f5296bf7625900
出典データセット
uspto-grants-2009_05
特許番号
US07528173B2

関連ノート

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