Hydrochloric Acid → 5-((6-(Trifluoromethyl)pyridin-3-yl)methoxy)pyridazin-3(2H)-one

HRID 474935노트

반응식

HRID 474935 반응식
O1CCCCC1[N:7]1[C:12](=[O:13])[CH:11]=[C:10]([O:14][CH2:15][C:16]2[CH:17]=[N:18][C:19]([C:22]([F:25])([F:24])[F:23])=[CH:20][CH:21]=2)[CH:9]=[N:8]1.Cl>CO.CCOCC>[F:25][C:22]([F:23])([F:24])[C:19]1[N:18]=[CH:17][C:16]([CH2:15][O:14][C:10]2[CH:9]=[N:8][NH:7][C:12](=[O:13])[CH:11]=2)=[CH:21][CH:20]=1

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 668688942-(Tetrahydro-2H-pyran-2-yl)-5-((6-(trifluoromethyl)pyridin-3-yl)methoxy)pyridazin-3(2H)-one

생성물 1

HCID 668688325-((6-(Trifluoromethyl)pyridin-3-yl)methoxy)pyridazin-3(2H)-one수율 67.6%

시약·촉매·용매 2

HCID 887Methanol용매HCID 3283Diethyl Ether용매2회

실험 절차

2-(Tetrahydro-2H-pyran-2-yl)-5-((6-(trifluoromethyl)pyridin-3-yl)methoxy)pyridazin-3(2H)-one (5.25 g, 12 mmol estimated) was stirred in MeOH (10 mL), and 2 N HCl in Et2O (50 mL) was added. After 16H, the mixture was diluted with Et2O (100 mL), and the solid was filtered off. The solid was stirred in NaHCO3 solution (15 mL) for 15 minutes and then refiltered to provide the title compound (2.2 g, 67%) as a white solid: 1H NMR (300 MHz, DMSO-d6) δ 12.74 (s, 1H), 8.78 (s, 1H), 8.20-8.16 (dd, J=8.1, 1.5 Hz, 1H), 8.00 (d, J=8.1 Hz, 1H), 7.76 (d, J=2.6 Hz, 1H), 6.31 (s, 1H), 5.25 (s, 2H).

후처리

  1. filtrationthe solid was filtered off

출처 및 근거

ORD 기록
ord-69a2aad1d20d4998a75d4ee92fae8caa
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08637501B2

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