p-Toluenesulfonic acid monohydrate → HCID 67868427、化合物

HRID 467289ノート

反応式

HRID 467289 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[NH:9][C:10]1[CH:15]=[CH:14][C:13]([OH:16])=[CH:12][C:11]=1[CH2:17][C:18]([OH:20])=[O:19].O.C1(C)C=CC(S(O)(=O)=O)=CC=1>CO>[C:18]([OH:20])(=[O:19])[CH3:17].[CH3:17][C:11]1[CH:12]=[C:13]([OH:16])[CH:14]=[CH:15][C:10]=1[NH:9][C:3]1[C:4]([Cl:8])=[CH:5][CH:6]=[CH:7][C:2]=1[Cl:1]

参加物

4

反応物 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 30525665-Hydroxydiclofenac

生成物 1

HCID 67868427HCID 67868427、化合物収率 90%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of the acid of Step E, above (2.0 g, 6.4 mmol) in 20 mL of methanol containing a few mg of p-toluene sulfonic acid monohydrate is heated at reflux for 3 hours. The solvent is evaporated in vacuo and the residue dissolved in ethyl acetate. The organic phase is washed with saturated NaHCO3, brine and dried (MgSO4). Removal of solvent affords the product (1.9 g, 90%) as a brown foam. It is used as such in the next step.

後処理

  1. temperatureat reflux for 3 hours
  2. customThe solvent is evaporated in vacuo
  3. dissolutionthe residue dissolved in ethyl acetate
  4. washThe organic phase is washed with saturated NaHCO3, brine
  5. dry with materialdried (MgSO4)
  6. customRemoval of solvent

出典と根拠

ORDレコード
ord-320cad30f9e642d0981bd5322cbbd22a
出典データセット
uspto-grants-1992_10
特許番号
US05159085

反応ノート

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