تفاعل #1797493

ord-7573a06fde9e4be5af8da2e0a35cb8d9

معادلة التفاعل

Nc1ccc2c(c1)CCC2
5-aminoindane
CC(=O)OC(C)=O
acetic anhydride
CC(=O)Nc1ccc2c(c1)CCC2
5-(N-acetylamino)indane
المردود 84.6%

المتفاعلات

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
50°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONAfter completion of the dropwise addition
  2. 2
    أخرىAfter completion of the reaction
  3. 3
    أخرىthe reaction liquid
  4. 4
    workup.STIRRINGwhile stirring
  5. 5
    أخرىCrystals precipitated
  6. 6
    ترشيحwere filtered off
  7. 7
    غسيلwashed with 1,000 ml of water
  8. 8
    أخرىThe crystals obtained
  9. 9
    أخرىwere dried

الإجراء التجريبي

33.3 g (0.25 mol) of 5-aminoindane (a product of Tokyo Chemical Industry Co. Ltd.) was dissolved in 250 ml of glacial acetic acid, the resulting solution was heated to 50° C., and 51.0 g (0.5 mol) of acetic anhydride was added dropwise thereto. After completion of the dropwise addition, the resulting solution was stirred for 4 hours. After completion of the reaction, the reaction liquid was poured in 1,500 ml of ice water while stirring. Crystals precipitated were filtered off, and washed with 1,000 ml of water. The crystals obtained were dried to obtain 37.06 g of 5-(N-acetylamino)indane (yield: 84.6%, melting point: 100.5 to 103.5° C.)

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07790342B2uspto-grants-2010_09