Реакция #2146772

ord-db3ce17cc06943ddb33cee7f153cd98b

Условия реакции

Температура
150°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.DISTILLATIONThen the excess trifluoroacetic acid was distilled off in vacuo
  2. 2
    workup.ADDITIONthe residue was diluted with 10 ml 1 M hydrochloric acid
  3. 3
    ПромывкаThe aqueous phase was washed with methylene chloride twice
  4. 4
    Другоеdried

Методика

0.53 g (1.1 mmol) (R)-3-[2-(4-Methoxy-benzyl)-7-methyl-1-oxo-1,2-dihydro-isoquinolin-6-yloxymethyl]-pyrrolidine-1-carboxylic acid tert-butyl ester were dissolved in 2.5 g (22 mmol) trifluoroacetic acid. After 1 h at room temperature the mixture was heated for 2 h in a microwave oven at 150° C. Then the excess trifluoroacetic acid was distilled off in vacuo and the residue was diluted with 10 ml 1 M hydrochloric acid. The aqueous phase was washed with methylene chloride twice and then it was freeze dried to give 0.11 g 7-Methyl-6-((R)-1-pyrrolidin-3-ylmethoxy)-2H-isoquinolin-1-one as the hydrochloride. Rt=0.82 min (Method B). Detected mass: 259.1 (M+H+).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08278294B2uspto-grants-2012_10