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Hydrochloric Acid → 8-(1-((3,5-difluorophenyl)(methyl)amino)ethyl)-2-morpholino-4-oxo-4H-chromene-6-carboxylic acid

HRID 1947343
ノート
印刷プレビュー

反応式

HRID 1947343 の反応式
[OH-].[Na+].[F:3][C:4]1[CH:5]=[C:6]([N:11]([CH3:35])[CH:12]([C:14]2[CH:15]=[C:16]([C:31]([O:33]C)=[O:32])[CH:17]=[C:18]3[C:23]=2[O:22][C:21]([N:24]2[CH2:29][CH2:28][O:27][CH2:26][CH2:25]2)=[CH:20][C:19]3=[O:30])[CH3:13])[CH:7]=[C:8]([F:10])[CH:9]=1.CO.Cl>C1COCC1.O>[F:3][C:4]1[CH:5]=[C:6]([N:11]([CH3:35])[CH:12]([C:14]2[CH:15]=[C:16]([C:31]([OH:33])=[O:32])[CH:17]=[C:18]3[C:23]=2[O:22][C:21]([N:24]2[CH2:29][CH2:28][O:27][CH2:26][CH2:25]2)=[CH:20][C:19]3=[O:30])[CH3:13])[CH:7]=[C:8]([F:10])[CH:9]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 14798Sodium HydroxideHCID 58235022methyl 8-(1-((3,5-difluorophenyl)(methyl)amino)ethyl)-2-morpholino-4-oxo-4H-chromene-6-carboxylate

生成物 1

HCID 582349758-(1-((3,5-difluorophenyl)(methyl)amino)ethyl)-2-morpholino-4-oxo-4H-chromene-6-carboxylic acid収率 86%

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 8028Tetrahydrofuran溶媒

実験手順

2N NaOH (6.54 mL, 13.1 mmol), was added dropwise to a stirred suspension of methyl 8-(1-((3,5-difluorophenyl)(methyl)amino)ethyl)-2-morpholino-4-oxo-4H-chromene-6-carboxylate (3 g, 6.54 mmol), in THF (30 mL)/MeOH (30 mL). The resulting solution was stirred at RT overnight. The reaction mixture was diluted with water, the pH was adjusted to 3 with a 2M aq. sol. HCl. The solvents were removed and the white precipitate was collected by filtration, washed with water and dried then washed with ethyl acetate and ether to afford 8-(1-((3,5-difluorophenyl)(methyl)amino)ethyl)-2-morpholino-4-oxo-4H-chromene-6-carboxylic acid (2.5 g, 86%) which was used without further purification. Mass Spectrum: M+H+ 445.

後処理

  1. customThe solvents were removed
  2. filtrationthe white precipitate was collected by filtration
  3. washwashed with water
  4. customdried
  5. washthen washed with ethyl acetate and ether

出典と根拠

ORDレコード
ord-e9ee0590372d4bb19e1d8175a9f392ea
出典データセット
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08399460B2

反応ノート

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