Acetic Acid → HCID 178525439、化合物

温度

80 °C

After 1.38 g (6.4 mmol) of ferrocene-aldehyde (Aldrich Corp) was dissolved in 20 mL of a DMF solution, the mixture was mixed with a solution of 0.75 g (5.7 mmol) of 6-amino caproic acid (Merck Corp.) in 5 mL of NaOH and refluxed at 80° C. for 2 hours. The reaction mixture was cooled to room temperature, and a solution of NaBH4 (0.63 g, 16.5 mmol) in 5 mL of water was added little by little into the reaction mixture (refer to FIG. 11). After 12 hours later, an aqueous acetic acid solution (10%) was slowly added until the pH reached 5. The reaction by-product ferrocene-CH2OH and unreacted 6-amino caproic acid dissolved in the organic phase was removed through extraction using ethylacetate. The aqueous phase was distilled at 50° C. under reduced pressure to obtain yellowish brown crystals. The yellowish brown crystals were recrystallized by dissolving the crystals in high-temperature ethanol to obtain planar, yellow crystalline N-(ferrocenyl methyl)-6-amino caproic acid.

1. temperatureThe reaction mixture was cooled to room temperature
2. customwas removed through extraction
3. distillationThe aqueous phase was distilled at 50° C. under reduced pressure
4. customto obtain yellowish brown crystals
5. customThe yellowish brown crystals were recrystallized
6. dissolutionby dissolving the crystals in high-temperature ethanol

ORDレコード

ord-c2e5a198e4eb4adda1d5c178e958d27f

出典データセット

uspto-grants-2009_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07479254B2