Acetic Acid → HCID 13347277, 화합물

HRID 1098762노트

반응식

HRID 1098762 반응식
[C:1]([C:4]1[CH:11]=[CH:10]C(C#N)=[C:6]([Br:12])[CH:5]=1)(=[O:3])[CH3:2].[OH-].[Na+].[CH3:15][C:16]([OH:18])=[O:17]>O.OS(O)(=O)=O>[C:1]([C:4]1[CH:11]=[CH:10][C:15]([C:16]([OH:18])=[O:17])=[C:6]([Br:12])[CH:5]=1)(=[O:3])[CH3:2]

참가 물질

6

반응물 3

HCID 176Acetic AcidHCID 14798Sodium HydroxideHCID 133472764-Acetyl-2-bromobenzonitrile

생성물 1

HCID 13347277HCID 13347277, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 1118Sulfuric Acid용매

실험 절차

A solution of the product obtained in step 2 (0.5 g, 2.23 mmol) in AcOH (2.5 mL), H2O (2.5 mL) and concentrated H2SO4 (2.5 mL) was refluxed for 5 h. After cooling, the reaction mixture was adjusted with 10 N NaOH to pH=10 and washed with AcOEt. The aqueous layer was acidified with concentrated HCl to pH=1 and then extracted with AcOEt. The organic phase was washed with H2O, dried over Na2SO4 and evaporated under reduced pressure. The crude product was used in the following step without further purification.

후처리

  1. temperatureAfter cooling
  2. washwashed with AcOEt
  3. extractionextracted with AcOEt
  4. washThe organic phase was washed with H2O
  5. dry with materialdried over Na2SO4
  6. customevaporated under reduced pressure
  7. customThe crude product was used in the following step without further purification

출처 및 근거

ORD 기록
ord-c1267523512b47bb811029123f96d168
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08143242B2

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