Hydrochloric Acid → HCID 22261126、化合物

HRID 1609978ノート

反応式

HRID 1609978 の反応式
C([O:3][C:4](=[O:30])[C:5]([CH3:29])([O:7][C:8]1[CH:13]=[CH:12][C:11]([S:14][CH2:15][CH2:16][C:17]2[N:18]=[C:19]([C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)[O:20][C:21]=2[CH3:22])=[CH:10][CH:9]=1)[CH3:6])C.[OH-].[Na+].Cl>CCO>[CH3:29][C:5]([O:7][C:8]1[CH:9]=[CH:10][C:11]([S:14][CH2:15][CH2:16][C:17]2[N:18]=[C:19]([C:23]3[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=3)[O:20][C:21]=2[CH3:22])=[CH:12][CH:13]=1)([CH3:6])[C:4]([OH:30])=[O:3]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 69313539HCID 69313539、化合物

生成物 1

HCID 22261126HCID 22261126、化合物収率 105%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

2-Methyl-2-{4-[2-(5-methyl-2-phenyl-oxazol-4-yl)ethylsulfanyl]phenoxy}propionic acid ethyl ester (98 mg, 0.23 mmol) was dissolved in EtOH (10 mL) and 5N NaOH (0.5 mL) was added. The reaction was stirred overnight at rt. The reaction was acidified with 5N HCl and the product was extracted into EtOAc, dried (MgSO4) and concentrated to give 96 mg crude product. Purification by reverse phase HPCL gave 47.5 mg (52%) as a light tan solid: mp 104-106° C., 1H NMR (DMSO-d6) δ 1.47 (s, 6H), 2.26 (s, 3H), 2.71 (t, 2H), 3.16 (t, 2H), 6.78 (d, 2H), 7.30 (d, 2H), 7.48 (m, 3H), 7.90 (m, 2H), 13.08 (br s, 1H).

後処理

  1. extractionthe product was extracted into EtOAc
  2. dry with materialdried (MgSO4)
  3. concentrationconcentrated

出典と根拠

ORDレコード
ord-16e81cca698f4f41892e74908f9366a7
出典データセット
uspto-grants-2006_01
特許番号
US06982278B2

反応ノート

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