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

HRID 1460632ノート

反応式

HRID 1460632 の反応式
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

参加物

6

反応物 3

HCID 7918Acetic AnhydrideHCID 517045Sodium AcetateHCID 45260987HCID 45260987、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 8857Ethyl Acetate溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-abacf55fdafc44d290373d267b861392
出典データセット
uspto-grants-1991_12
特許番号
US05071875

反応ノート

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