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Hydrochloric Acid → HCID 57486101、化合物

HRID 421167
ノート
印刷プレビュー

反応式

HRID 421167 の反応式
C[O:2][C:3](=[O:27])[CH2:4][C:5]1[S:9][C:8]([NH:10][C:11](=[O:20])[C:12]2[CH:17]=[C:16]([Br:18])[CH:15]=[CH:14][C:13]=2[OH:19])=[N:7][C:6]=1[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.[OH-].[Na+].Cl>CO>[Br:18][C:16]1[CH:15]=[CH:14][C:13]([OH:19])=[C:12]([CH:17]=1)[C:11]([NH:10][C:8]1[S:9][C:5]([CH2:4][C:3]([OH:27])=[O:2])=[C:6]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[N:7]=1)=[O:20]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 86595540HCID 86595540、化合物

生成物 1

HCID 57486101HCID 57486101、化合物収率 77.3%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

{2-[(5-Bromo-2-hydroxybenzoyl)amino]-4-phenylthiazol-5-yl}acetic acid methyl ester (75 mg, 0.17 mmol) was dissolved in methanol (5 mL). 2 N sodium hydroxide (0.5 mL, 1 mmol) was added, and the mixture was stirred at room temperature for 12 hours. The reaction mixture was poured into 2 N hydrochloric acid and extracted with ethyl acetate. After the ethyl acetate layer was washed with water and brine one after another, dried over anhydrous sodium sulfate, the solvent was evaporated under reduced pressure. The obtained residue was suspended and washed with n-hexane-ethyl acetate under heating at reflux to give the title compound (56 mg, 77.3%) as a light yellow white crystal.

後処理

  1. extractionextracted with ethyl acetate
  2. washAfter the ethyl acetate layer was washed with water and brine one after another,
  3. dry with materialdried over anhydrous sodium sulfate
  4. customthe solvent was evaporated under reduced pressure
  5. washwashed with n-hexane-ethyl acetate
  6. temperatureunder heating
  7. temperatureat reflux

出典と根拠

ORDレコード
ord-5f8cd8a2652f46d48a6066f204d19eda
出典データセット
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08097759B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート