Water → 2-Cyclobutoxy-5-hydroxymethyl-3-methyl-benzoic acid

HRID 1047895노트

반응식

HRID 1047895 반응식
C[O:2][C:3](=[O:18])[C:4]1[CH:9]=[C:8]([CH2:10][OH:11])[CH:7]=[C:6]([CH3:12])[C:5]=1[O:13][CH:14]1[CH2:17][CH2:16][CH2:15]1.[OH-].[K+].O>CCO>[CH:14]1([O:13][C:5]2[C:6]([CH3:12])=[CH:7][C:8]([CH2:10][OH:11])=[CH:9][C:4]=2[C:3]([OH:18])=[O:2])[CH2:17][CH2:16][CH2:15]1

참가 물질

5

반응물 3

HCID 962WaterHCID 14797Potassium HydroxideHCID 593140822-Cyclobutoxy-5-hydroxymethyl-3-methyl-benzoic acid methyl ester

생성물 1

HCID 593143012-Cyclobutoxy-5-hydroxymethyl-3-methyl-benzoic acid수율 100%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

2-Cyclobutoxy-5-hydroxymethyl-3-methyl-benzoic acid methyl ester (410 mg, 1.64 mmol) is dissolved in EtOH (15 mL), and solid KOH (1.90 g, 32.8 mmol) and water (1.5 mL) are added. The mixture is stirred at RT for 1 h then concentrated in vacuo. The residue is dissolved in water (10 mL) and acidified with conc. HCl then extracted with EtOAc (3×10 mL). The combined organic layers are dried over anhydrous MgSO4 and concentrated in vacuo to give product (284) as viscous yellow oil (387 mg, 100%).

후처리

  1. concentrationthen concentrated in vacuo
  2. dissolutionThe residue is dissolved in water (10 mL)
  3. extractionthen extracted with EtOAc (3×10 mL)
  4. dry with materialThe combined organic layers are dried over anhydrous MgSO4
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-6e93bfb7b7c149958716ce3e5bb9be81
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08569535B2

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