Hydrochloric Acid → HCID 11612836、化合物

HRID 2355126ノート

反応式

HRID 2355126 の反応式
[CH3:1][N:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4]([C:11]2[O:12][C:13]([C:16]3[CH:17]=[C:18]4[C:23](=[CH:24][CH:25]=3)[CH:22]=[C:21]([O:26][CH:27]([CH2:32][C:33]3[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=3)[C:28]([O:30]C)=[O:29])[CH:20]=[CH:19]4)=[CH:14][N:15]=2)=[CH:3]1.[OH-].[Na+].Cl>C1COCC1.CO.O>[CH3:1][N:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4]([C:11]2[O:12][C:13]([C:16]3[CH:17]=[C:18]4[C:23](=[CH:24][CH:25]=3)[CH:22]=[C:21]([O:26][CH:27]([CH2:32][C:33]3[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=3)[C:28]([OH:30])=[O:29])[CH:20]=[CH:19]4)=[CH:14][N:15]=2)=[CH:3]1

参加物

7

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 68452478HCID 68452478、化合物

生成物 1

HCID 11612836HCID 11612836、化合物収率 90%

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of methyl 2-({6-[2-(1-methyl-1H-indol-3-yl)-1,3-oxazol-5-yl]-2-naphthyl}oxy)-3-phenylpropanoate (185 mg, 0.369 mmol), prepared in the previous step, and 1 N NaOH (550 μL, 0.55 mmol) in 10 mL of THF, 10 mL of methanol and 5 mL of H2O was stirred at room temperature for 18 h (overnight). The reaction was acidified by the addition of 600μL of 1N HCl and then concentrated under reduced pressure to remove the THF and the methanol. The white solid that formed was collected by filtration, rinsed with water and dried under reduced pressure to give the title compound (102 mg, 90%) as a white solid, mp 149-151° C. Elemental Analysis for C31H24N2O4+0.36 H2O Calc'd: C, 75.22; H, 5.03; N, 5.66. Found: C, 75.28 ;H, 5.22; N, 5.39.

後処理

  1. concentrationconcentrated under reduced pressure
  2. customto remove the THF
  3. customThe white solid that formed
  4. filtrationwas collected by filtration
  5. washrinsed with water
  6. customdried under reduced pressure

出典と根拠

ORDレコード
ord-7b7f8e4595204b38aeb563effd59ab7c
出典データセット
uspto-grants-2010_07
特許番号
US07754747B2

反応ノート

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