反应 #1340582

ord-8d6007077784428b8f31c7e3d6b9d121

反应方程式

O=C(O)CCSSCCC(=O)O
3,3′-dithiodipropionic acid
CS(=O)(=O)O
methanesulfonic acid
CCN(CC)CCCCCCO
6-(N,N-diethyl)amino-1-hexanol
CCN(CC)CCCCCCOC(=O)CCSSCCC(=O)OCCCCCCN(CC)CC
di[6-(N,N-diethyl)aminohexyl]3,3′-dithiodipropionate

反应条件

温度
120°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他completion of the reaction
  2. 2
    温度the reaction mixture was cooled to room temperature
  3. 3
    workup.STIRRINGAfter stirring for 2 hours
  4. 4
    过滤the precipitated crystals were collected by filtration
  5. 5
    洗涤washed with acetone

实验过程

1.3 g of methanesulfonic acid (manufactured by Wako Pure Chemical Industries, Ltd.) was added dropwise, under an atmosphere of nitrogen and at 70° C., to 2.3 g of the obtained 6-(N,N-diethyl)amino-1-hexanol. After stifling for 10 minutes, 1.4 g of 3,3′-dithiodipropionic acid (manufactured by Wako Pure Chemical Industries, Ltd.) was added, and the resulting mixture was heated to 120° C. and then stirred at 110° C. for 4 hours. Following completion of the reaction, the reaction mixture was cooled to room temperature and then added gradually to 50 mL of methyl isobutyl ketone (manufactured by Wako Pure Chemical Industries, Ltd.). After stirring for 2 hours, the precipitated crystals were collected by filtration and washed with acetone, yielding the methanesulfonate salt of di[6-(N,N-diethyl)aminohexyl]3,3′-dithiodipropionate.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08455413B2uspto-grants-2013_06