تفاعل #721149

ord-26655889aa714c4e94f0ebb396627753

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    تركيزconcentrated to dryness
  2. 2
    workup.STIRRINGAfter 10 minutes stirring at room temperature
  3. 3
    ترشيحthe precipitate was filtered
  4. 4
    غسيلwashed with diethyl ether

الإجراء التجريبي

Trifluoroacetic acid (1 mL) was added to a suspension of (E)-tert-butyl 3-(4(4-methoxybenzyl)-2-oxo-2,3,4,5-tetrahydro-1H-pyrido[2,3-e][1,4]diazepin-7-yl)acrylate (112 mg, 0.27 mmol) in dichloromethane (1 mL) at room temperature. The reaction mixture was then stirred for 1 hour and concentrated to dryness. The resulting residue was suspended in a solution of hydrochloric acid in dioxane 4N (2 mL). After 10 minutes stirring at room temperature, the precipitate was filtered and washed with diethyl ether to afford the title product as a pale yellow solid (110 mg, quantitative).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09321769B2uspto-grants-2016_04