Hydrochloric Acid → HCID 59800131, 화합물

150 g (519 mmol) of N-Boc-5-ethoxycarbonylindole and 192 ml (833 mmol) of triisopropyl borate in 350 ml of toluene were admixed at from 5° C. to 10° C. with 350 ml of a 1.8 molar solution of LDA in THF. The mixture was stirred for a further 5 min and the reaction mixture was added to a solution of 278 g of 30% hydrochloric acid and 940 ml of water. Subsequently, the mixture was stirred at from 5° C. to 10° C. for 30 min. Thereafter, the mixture was filtered and the filtercake was suspended in 530 ml of ethanol. This suspension was added at 40° C. to a solution of 500 ml of 30% hydrochloric acid and 224 ml of ethanol. Subsequently, the mixture was stirred at from 40° C. to 45° C. for 2.5 h and admixed at 30° C. with 380 ml of water. The mixture was then cooled to from 10° C. to 15° C., stirred at this temperature for 30 min and filtered. Drying under reduced pressure afforded 79.5 g (61% of theory) of 2-borono-5-ethoxycarbonylindole (HPLC: 92.7 area %).

1. stirringSubsequently, the mixture was stirred at from 5° C. to 10° C. for 30 min
2. filtrationThereafter, the mixture was filtered
3. additionThis suspension was added at 40° C. to a solution of 500 ml of 30% hydrochloric acid and 224 ml of ethanol
4. stirringSubsequently, the mixture was stirred at from 40° C. to 45° C. for 2.5 h
5. customadmixed at 30° C. with 380 ml of water
6. temperatureThe mixture was then cooled to from 10° C. to 15° C.
7. stirringstirred at this temperature for 30 min
8. filtrationfiltered
9. customDrying under reduced pressure

ORD 기록

ord-7648514ede3f49818adb6c40830c2fa9

출처 데이터셋

uspto-grants-2012_07

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US08232395B2