HCID 59627701, 화합물 → HCID 59627640, 화합물

HRID 1930117노트

반응식

HRID 1930117 반응식
[Cl:1][C:2]1[C:3]([O:16][CH3:17])=[CH:4][C:5]([CH3:15])=[C:6]([C:8](=[O:14])[C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH:7]=1>CC(O)=O.[Zn]>[Cl:1][C:2]1[C:3]([O:16][CH3:17])=[CH:4][C:5]([CH3:15])=[C:6]([CH:8]([OH:14])[C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH:7]=1

참가 물질

4

반응물 1

HCID 59627701HCID 59627701, 화합물2회

생성물 1

HCID 59627640HCID 59627640, 화합물수율 92.4%

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 176Acetic Acid용매2회

실험 절차

A solution of ethyl 2-(5-chloro-4-methoxy-2-methylphenyl)-2-oxoacetate (Intermediate 3-7; 6.12 g, 23.84 mmol) in warm AcOH (60 mL) was added to a stirred suspension of zinc dust (7.80 g, 119.21 mmol) in AcOH (20 mL) and the resulting suspension was stirred at ambient temperature for 16 hours. The reaction mixture was filtered, the filtrate diluted with EtOAc (200 mL), and washed with saturated brine (3×125 mL). The organic layer was dried over MgSO4, filtered and evaporated to afford ethyl 2-(5-chloro-4-methoxy-2-methylphenyl)-2-hydroxyacetate (5.70 g, 92%) as a pale yellow oil which solidified on standing, which was used without further purification.

후처리

  1. filtrationThe reaction mixture was filtered
  2. additionthe filtrate diluted with EtOAc (200 mL)
  3. washwashed with saturated brine (3×125 mL)
  4. dry with materialThe organic layer was dried over MgSO4
  5. filtrationfiltered
  6. customevaporated

출처 및 근거

ORD 기록
ord-43398da6e19146bba0df727dbd9a353c
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08188092B2

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