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Hydrochloric Acid → 4-[2-(5-Chloro-2-hydroxybenzoylamino)benzoylamino]butanoic acid

HRID 2374718
ノート
印刷プレビュー

反応式

HRID 2374718 の反応式
[NH2:1][C:2]1[CH:16]=[CH:15][CH:14]=[CH:13][C:3]=1[C:4]([NH:6][CH2:7][CH2:8][CH2:9][C:10]([OH:12])=[O:11])=[O:5].C[Si](Cl)(C)C.C(N(CC)CC)C.[Cl:29][C:30]1[CH:31]=[CH:32][C:33]([OH:39])=[C:34]([CH:38]=1)[C:35](Cl)=[O:36].[OH-].[Na+].Cl>C(Cl)Cl>[Cl:29][C:30]1[CH:31]=[CH:32][C:33]([OH:39])=[C:34]([CH:38]=1)[C:35]([NH:1][C:2]1[CH:16]=[CH:15][CH:14]=[CH:13][C:3]=1[C:4]([NH:6][CH2:7][CH2:8][CH2:9][C:10]([OH:12])=[O:11])=[O:5])=[O:36]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 6

HCID 313Hydrochloric AcidHCID 6397ChlorotrimethylsilaneHCID 8471TriethylamineHCID 14798Sodium HydroxideHCID 128632335-Chloro-2-hydroxybenzoyl chlorideHCID 134423754-(2-Aminobenzamido)butanoic acid

生成物 1

HCID 23118566
4-[2-(5-Chloro-2-hydroxybenzoylamino)benzoylamino]butanoic acid

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a suspension of 2.30 g (10.4 mmol) of 4-(2-aminobenzoylamino)butanoic acid in 40 ml of dry methylene chloride, add 9.56 g (88.50 mmol) of trimethylsilyl chloride and allow the reaction to reflux for 5 hours. Then place the flask in an ice bath and add 1.34 g (13.30 mmol) of triethylamine and a solution of 1.67 g (8.85 mmol) of 5-chloro-2-hydroxybenzoyl chloride dissolved in 5 ml of dry methylene chloride. Allow the reaction to stir for 30 minutes in an ice bath and 24 hours at room temperature. Eliminate the solvent at low pressure, add 30 ml of 10% NaOH to the crude product and continue stirring the mixture until the oil has completely disappeared. Immediately acidify with concentrated HCl, filter the resulting solid and wash several times with water and with ether. Purify the reaction product by recrystallization (EtOH/H2O). This yields 0.95 g (29%) of 4-[2-(5-chloro-2-hydroxybenzoylamino)benzoylamino]butanoic acid as a white solid.

後処理

  1. customthe reaction
  2. temperatureto reflux for 5 hours
  3. customthe reaction
  4. stirringcontinue stirring the mixture until the oil
  5. filtrationfilter the resulting solid
  6. washwash several times with water
  7. customPurify the reaction product
  8. customby recrystallization (EtOH/H2O)

出典と根拠

ORDレコード
ord-133efa7cc3114b5d8a5d52402b5a2804
出典データセット
uspto-grants-2008_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07462735B2

反応ノート

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