Acetic Anhydride → Acetamide, N-(1,2,3,4-tetrahydro-4-phenyl-2-naphthalenyl)-

HRID 1460632노트

반응식

HRID 1460632 반응식
Cl.[C:2]1([CH:8]2[C:17]3[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=3)[CH2:11][CH:10]([NH2:18])[CH2:9]2)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:19]([O-])(=[O:21])[CH3:20].[Na+].C(OC(=O)C)(=O)C>C(OCC)(=O)C.O>[C:2]1([CH:8]2[C:17]3[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=3)[CH2:11][CH:10]([NH:18][C:19](=[O:21])[CH3:20])[CH2:9]2)[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

6

반응물 3

HCID 7918Acetic AnhydrideHCID 517045Sodium AcetateHCID 45260987HCID 45260987, 화합물

생성물 1

HCID 10220953Acetamide, N-(1,2,3,4-tetrahydro-4-phenyl-2-naphthalenyl)-수율 80.1%

시약·촉매·용매 2

HCID 962Water용매2회HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 180 mg (0.80 mmol) of 4-phenyl-2-aminotetraline HCl in 3.5 ml ethyl acetate and 2.0 ml water, was added 360 mg of sodium acetate. To this mixture 0.6 ml of acetic anhydride was then added and the mixture was stirred for 24 hrs. The addition of 2 ml of water resulted in the formation of two layers. After separation, the water layer was extracted twice with ethyl acetate. The combined organic layers were washed 3 times with a saturated solution of sodium bicarbonate and once with a saturated solution of sodium chloride. After drying over magnesium sulfate, the organic solution was evaporated under reduced pressure to yield 4-phenyl-2-acetamidotetralin as a white solid (170 mg, 79%).

후처리

  1. customresulted in the formation of two layers
  2. customAfter separation
  3. extractionthe water layer was extracted twice with ethyl acetate
  4. washThe combined organic layers were washed 3 times with a saturated solution of sodium bicarbonate
  5. dry with materialAfter drying over magnesium sulfate
  6. customthe organic solution was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-abacf55fdafc44d290373d267b861392
출처 데이터셋
uspto-grants-1991_12
특허 번호
US05071875

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