تفاعل #1340581

ord-5032cbba7aaf45d4a4653b80204863c5

معادلة التفاعل

O=C(O)CCSSCCC(=O)O
3,3′-dithiodipropionic acid
CS(=O)(=O)O
methanesulfonic acid
NCCCCCCO
6-amino-1-hexanol
NCCCCCCOC(=O)CCSSCCC(=O)OCCCCCCN
di(6-aminohexyl) 3,3′-dithiodipropionate

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
120°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.STIRRINGstirred at 110° C. for 3 hours
  2. 2
    أخرىcompletion of the reaction
  3. 3
    درجة الحرارةthe reaction mixture was cooled to room temperature
  4. 4
    workup.STIRRINGAfter stirring for 2 hours
  5. 5
    ترشيحthe precipitated crystals were collected by vacuum filtration
  6. 6
    غسيلwashed with acetone

الإجراء التجريبي

2.0 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 6-amino-1-hexanol (manufactured by Tokyo Chemical Industry Co., Ltd.). After stirring for 10 minutes, 2.1 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 3 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 vacuum filtration and washed with acetone, yielding the methanesulfonate salt of di(6-aminohexyl) 3,3′-dithiodipropionate.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08455413B2uspto-grants-2013_06