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Water → 4-Bromo-2-(methylsulfonamido)benzoic acid

HRID 2411352
ノート
印刷プレビュー

反応式

HRID 2411352 の反応式
[NH2:1][C:2]1[CH:11]=[C:10]([Br:12])[CH:9]=[CH:8][C:3]=1[C:4]([O:6]C)=[O:5].C(N(CC)CC)C.[CH3:20][S:21](Cl)(=[O:23])=[O:22].O>O1CCCC1>[Br:12][C:10]1[CH:9]=[CH:8][C:3]([C:4]([OH:6])=[O:5])=[C:2]([NH:1][S:21]([CH3:20])(=[O:23])=[O:22])[CH:11]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 17871390Methyl 2-Amino-4-bromobenzoate

生成物 1

HCID 226210824-Bromo-2-(methylsulfonamido)benzoic acid

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Methyl 2-amino-4-bromobenzoate (1 g) was dissolved in tetrahydrofuran (15 mL), triethylamine (4.2 mL) and methanesulfonyl chloride (0.74 mL) were added, and the mixture was stirred at room temperature for 6 hr. Water was added to the reaction mixture, and the mixture was extracted with chloroform. After evaporation of the solvent, to the residue were added methanol (20 mL) and 1N aqueous sodium hydroxide solution (13 mL), and the mixture was stirred at 50-60° C. After neutralizing with 1N hydrochloric acid, the precipitated solid was collected by filtration to give the title compound (964 mg).

後処理

  1. extractionthe mixture was extracted with chloroform
  2. customAfter evaporation of the solvent
  3. additionto the residue were added methanol (20 mL) and 1N aqueous sodium hydroxide solution (13 mL)
  4. stirringthe mixture was stirred at 50-60° C
  5. filtrationthe precipitated solid was collected by filtration

出典と根拠

ORDレコード
ord-9508b847c23b401ea2a18cf38e45e780
出典データセット
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08816079B2

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