Lithium Hydroxide → HCID 21942564, 화합물

HRID 2216763노트

반응식

HRID 2216763 반응식
[C:1]([C:3]1[CH:4]=[C:5]([CH:10]=[C:11]([O:13][CH2:14][CH2:15][O:16][CH3:17])[CH:12]=1)[C:6]([O:8]C)=[O:7])#[N:2].[OH-].[Li+]>O1CCCC1>[C:1]([C:3]1[CH:4]=[C:5]([CH:10]=[C:11]([O:13][CH2:14][CH2:15][O:16][CH3:17])[CH:12]=1)[C:6]([OH:8])=[O:7])#[N:2]

참가 물질

4

반응물 2

HCID 3939Lithium HydroxideHCID 21942473Benzoic acid, 3-cyano-5-(2-methoxyethoxy)-, methyl ester

생성물 1

HCID 21942564HCID 21942564, 화합물수율 97%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
70 °C

실험 절차

A solution of methyl 3-cyano-5-(2-methoxyethoxy)benzoate (375 mg, 1.6 mmol) in tetrahydrofuran (4 mL) was treated with 0.5 N lithium hydroxide (3.8 mL, 1.9 mmol). The reaction was stirred at 70° C. for 30 minutes and then the solvent was removed in vacuo. The residue was dissolved in a small amount of water and then acidified with 2 N hydrogen chloride until pH˜2. Following extraction of the aqueous layer with ethyl acetate, the organic layer washed with water and saturated brine, dried over anhydrous sodium sulfate, filtered, and concentrated to afford 343 mg (97%) of 3-cyano-5-(2-methoxyethoxy)benzoic acid.

후처리

  1. customthe solvent was removed in vacuo
  2. dissolutionThe residue was dissolved in a small amount of water
  3. extractionextraction of the aqueous layer with ethyl acetate
  4. washthe organic layer washed with water and saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-261a50b042194cf4845b5f281c23f796
출처 데이터셋
uspto-grants-2006_09
특허 번호
US07112595B2

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