Реакция #1340584

ord-1477f1b097fe4093b22526e1171ef0a6

Уравнение реакции

O=C(O)CCSSCCC(=O)O
3,3′-dithiodipropionic acid
CS(=O)(=O)O
methanesulfonic acid
CCCCC(N)CO
2-amino-1-hexanol
CCCCC(N)COC(=O)CCSSCCC(=O)OCC(N)CCCC
di(2-aminohexyl) 3,3′-dithiodipropionate

Растворители

Условия реакции

Температура
120°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеcompletion of the reaction
  2. 2
    Температураthe reaction mixture was cooled to room temperature
  3. 3
    workup.WAITAfter stifling for 1 hour
  4. 4
    Фильтрацияthe precipitated crystals were collected by filtration
  5. 5
    Другоеdried at 50° C.

Методика

6.1 g of methanesulfonic acid (manufactured by Wako Pure Chemical Industries, Ltd.) was added dropwise, under an atmosphere of nitrogen and at 70° C., to 7.0 g of 2-amino-1-hexanol (manufactured by Aldrich Co., Ltd.). After stifling for 10 minutes, 6.3 g of 3,3′-dithiodipropionic acid (manufactured by Wako Pure Chemical Industries, Ltd.) was added, and the resulting mixture was heated to 120° C. The mixture was then stirred at 120 to 129° C. for a further 3 hours. Following completion of the reaction, the reaction mixture was cooled to room temperature and then added gradually to 100 mL of methyl isobutyl ketone (manufactured by Wako Pure Chemical Industries, Ltd.). After stifling for 1 hour, the precipitated crystals were collected by filtration and dried at 50° C., yielding the methanesulfonate salt of di(2-aminohexyl) 3,3′-dithiodipropionate.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08455413B2uspto-grants-2013_06