p-Toluenesulfonic acid monohydrate → HCID 67868427, 화합물

HRID 467289노트

반응식

HRID 467289 반응식
[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]

참가 물질

4

반응물 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 30525665-Hydroxydiclofenac

생성물 1

HCID 67868427HCID 67868427, 화합물수율 90%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-320cad30f9e642d0981bd5322cbbd22a
출처 데이터셋
uspto-grants-1992_10
특허 번호
US05159085

반응 노트

불러오는 중…