Sulfuric Acid → HCID 178527055, 화합물

HRID 490925

반응식

HRID 490925 반응식
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

참가 물질

7

반응물 5

HCID 1118Sulfuric AcidHCID 2130AmantadineHCID 6547AzobisisobutyronitrileHCID 130333-ButenylbenzeneHCID 178418950HCID 178418950, 화합물

생성물 1

HCID 178527055HCID 178527055, 화합물수율 54.5%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-52c6bf5ce5e24e2cb1f5296bf7625900
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07528173B2

연결된 노트

불러오는 중…