反应 #1340580

ord-e1b75d5ab25b4a16bf3f81cf6cb00ff1

反应方程式

O=C(O)CCSCCC(=O)O
3,3′-thiodipropionic acid
CS(=O)(=O)O
methanesulfonic acid
NCCCCCCO
6-amino-1-hexanol
NCCCCCCOC(=O)CCSCCC(=O)OCCCCCCN
di(6-aminohexyl) 3,3′-thiodipropionate

反应条件

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

后处理

  1. 1
    workup.STIRRINGstirred at 110° C. for 7 hours
  2. 2
    其他completion of the reaction
  3. 3
    温度the reaction mixture was cooled to room temperature
  4. 4
    workup.STIRRINGAfter stirring for 2 hours
  5. 5
    过滤the precipitated crystals were collected by filtration
  6. 6
    洗涤washed with acetone

实验过程

8.1 g of methanesulfonic acid (manufactured by Wako Pure Chemical Industries, Ltd.) was added dropwise, under an atmosphere of nitrogen and at 70° C., to 9.4 g of 6-amino-1-hexanol (manufactured by Tokyo Chemical Industry Co., Ltd.). After stirring for 10 minutes, 7.1 g of 3,3′-thiodipropionic 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 7 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-aminohexyl) 3,3′-thiodipropionate.

来源

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