Triethylamine → HCID 86723565、化合物

Compound 8-3 (9.5 g, 0.068 mol) was dissolved in 300 mL of THF, and lithium aluminium hydride (2.62 g, 0.069 mol) was added slowly at −10° C. After the addition, reacted at room temperature for 2 hours, and added 5 mL of water after completion of the reaction of raw materials, suction filtered through Celite and the filtrate was concentrated to give an oil. The obtained oil and triethylamine (10.7 mL, 0.075 mol) were dissolved in 100 mL of DCM, and added dropwise benzyl chloroformate (11.6 g, 0.068 mol) slowly at −10° C., then further reacted for 2 hours at room temperature after the addition was completed. The reaction mixture was washed with 100 mL of water and 100 mL of saturated brine once respectively, dried and concentrated and purified by column chromatography (petroleum ether/ethyl acetate=10:1) to give Compound 8-4 as a white solid (6.3 g, yield 35.7%).

1. additionAfter the addition
2. customreacted at room temperature for 2 hours
3. customafter completion of the reaction of raw materials, suction
4. filtrationfiltered through Celite
5. concentrationthe filtrate was concentrated
6. customto give an oil
7. customfurther reacted for 2 hours at room temperature
8. additionafter the addition
9. washThe reaction mixture was washed with 100 mL of water and 100 mL of saturated brine once respectively
10. customdried
11. concentrationconcentrated
12. custompurified by column chromatography (petroleum ether/ethyl acetate=10:1)

ORDレコード

ord-f2caf040569a4134b7b4fc156e03985e

出典データセット

uspto-grants-2016_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09365499B2