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

HRID 474935ノート

反応式

HRID 474935 の反応式
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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 3283Diethyl Ether溶媒2 回

実験手順

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).

後処理

  1. filtrationthe solid was filtered off

出典と根拠

ORDレコード
ord-69a2aad1d20d4998a75d4ee92fae8caa
出典データセット
uspto-grants-2014_01
特許番号
US08637501B2

反応ノート

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