Lithium Hydroxide → 6-(Tert-butoxy)-6-oxohexanoic acid

HRID 331540

반응식

HRID 331540 반응식
[OH-].[Li+].C[O:4][C:5](=[O:17])[CH2:6][CH2:7][CH2:8][CH2:9][C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11]>CO.O>[C:13]([O:12][C:10](=[O:11])[CH2:9][CH2:8][CH2:7][CH2:6][C:5]([OH:17])=[O:4])([CH3:16])([CH3:14])[CH3:15]

참가 물질

4

반응물 2

HCID 3939Lithium HydroxideHCID 184750351-(1,1-Dimethylethyl) 6-methyl hexanedioate

생성물 1

HCID 159089376-(Tert-butoxy)-6-oxohexanoic acid수율 89.9%

시약·촉매·용매 1

HCID 22242641Methanol--water (1/1)용매

실험 절차

Lithium hydroxide (0.53 g, 22 mmol) was added to a solution of hexanedioic acid tert-butyl ester methyl ester (4.8 g, 22 mmol) in 3:1 methanol-water (80 mL), and the resulting mixture was stirred at room temperature for 16 hours. The mixture was evaporated under vacuum. The residue was partitioned between water (60 mL) and methylene chloride (75 mL), and the aqueous phase was washed with methylene chloride (3×75 mL) and evaporated, providing 4.0 g of hexanedioic acid mono-tert-butyl ester, lithium salt; 1H NMR (D2O) δ 1.45 (s, 9H), 1.54-1.58 (m, 4H), 2.15-2.20 (m, 2H), 2.25-2.34 (m, 2H).

후처리

  1. customThe mixture was evaporated under vacuum
  2. customThe residue was partitioned between water (60 mL) and methylene chloride (75 mL)
  3. washthe aqueous phase was washed with methylene chloride (3×75 mL)
  4. customevaporated

출처 및 근거

ORD 기록
ord-0c8b0c57370c4c28afc7cb9d2a04bc14
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08877780B2

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