Реакция #2146774

ord-0fa6ffc9093d4ac89e05ed27a49ba742

Уравнение реакции

COc1ccc(Cn2ccc3cc(O[C@@H]4CCNC4)c(C)cc3c2=O)cc1.Cl
2-(4-Methoxy-benzyl)-7-methyl-6-((R)-pyrrolidin-3-yloxy)-2H-isoquinolin-1-one hydrochloride
O=C(O)C(F)(F)F
trifluoroacetic acid
Cc1cc2c(=O)[nH]ccc2cc1OC[C@@H]1CCNC1.Cl
7-Methyl-6-((R)-1-pyrrolidin-3-ylmethoxy)-2H-isoquinolin-1-one hydrochloride
Выход 74.4%

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

245 mg of 2-(4-Methoxy-benzyl)-7-methyl-6-((R)-pyrrolidin-3-yloxy)-2H-isoquinolin-1-one hydrochloride were dissolved in 1.4 g trifluoroacetic acid and 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 134 mg 7-Methyl-6-((R)-1-pyrrolidin-3-ylmethoxy)-2H-isoquinolin-1-one hydrochloride. Rt=0.92 min (Method B). Detected mass: 245.1 (M+H+).

Источник

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