تفاعل #992697

ord-cb5847bc2b8849bfbcea377930f23d20

معادلة التفاعل

Nc1ccccc1
aniline
O=C(Cl)c1cccc2ccccc12
1-naphthoyl chloride
O
water
[NH4+].[OH-]
ammonium hydroxide
O=C(Nc1ccccc1)c1cccc2ccccc12
solid
المردود 82.0%
O=C(Nc1ccccc1)c1cccc2ccccc12
Naphthalene-1-carboxylic acid phenylamide
المردود 82.0%

الكواشف

لا شيء

ظروف التفاعل

درجة الحرارة
82°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىTo the solution so formed
  2. 2
    أخرى20 min
  3. 3
    أخرىThe phases were separated
  4. 4
    غسيلthe aqueous phase was washed with 100 ml of dichloromethane
  5. 5
    أخرىThe organic fractions were collected
  6. 6
    تجفيفdried with magnesium sulfate
  7. 7
    ترشيحfiltered
  8. 8
    أخرىthe solvent was then removed under reduced pressure

الإجراء التجريبي

4.77 g of 1-naphthoyl chloride (TCI America) was dissolved in 100 ml of anhydrous acetonitrile. To the solution so formed, 2.28 ml of aniline (Sigma-Aldrich) was added in a dropwise fashion over a period of c.a. 20 min. The reaction was then refluxed for 2 h at 82° C. 100 ml of distilled water and 5 ml of concentrated ammonium hydroxide were added along with 100 ml of diethyl ether in a separatory funnel. The phases were separated and the aqueous phase was washed with 100 ml of dichloromethane. The organic fractions were collected and dried with magnesium sulfate, filtered and the solvent was then removed under reduced pressure to yield a white solid 5.07 g (82%; 20.5 mmol).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08012458B2uspto-grants-2011_09