Hydrochloric Acid → 1,3-Bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane dihydrochloride

In a 500 ml four-necked flask equipped with a stirrer, a thermometer, a condenser, and a dropping funnel was placed 24.9 g (0.1 mole) of 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane having a gas chromatography purity of 98.4%. 31.3 g (0.3 mole) of concentrated hydrochloric acid was dropwise added to the flask, and the resulting mixture was stirred at room temperature for 30 minutes. 300 g of isopropanol was added to the solution. The resulting mixture was heated under reduced pressure, and isopropanol was distilled off while conducting azeotropic distillation, to obtain a concentrated and dried product. The concentrated and dried product thus obtained was recrystallized from isopropanol to obtain 28.9 g (yield: 90%) of 1,3-bis(3-amino-propyl)-1,1,3,3-tetramethyldisiloxane dihydrochloride which is an acid addition salt.

1. customIn a 500 ml four-necked flask equipped with a stirrer
2. distillationwas distilled off
3. distillationdistillation
4. customto obtain
5. concentrationa concentrated
6. concentrationThe concentrated
7. customdried product thus obtained
8. customwas recrystallized from isopropanol

ORDレコード

ord-3ee4890127fa4b50a6a7a34191b47ece

出典データセット

uspto-grants-1999_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05861085