Potassium Hydroxide → 2-(Hydroxymethyl)-5-methylbenzoic acid

HRID 2361332

반응식

HRID 2361332 반응식
[CH3:1][C:2]1[CH:10]=[C:9]2[C:5]([CH2:6][O:7][C:8]2=[O:11])=[CH:4][CH:3]=1.[OH-:12].[K+]>CO.O>[OH:12][CH2:6][C:5]1[CH:4]=[CH:3][C:2]([CH3:1])=[CH:10][C:9]=1[C:8]([OH:7])=[O:11]

참가 물질

5

반응물 2

HCID 14797Potassium HydroxideHCID 6387566-Methylphthalide

생성물 1

HCID 679628172-(Hydroxymethyl)-5-methylbenzoic acid수율 59.4%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

A colorless, homogeneous solution of 6-methylisobenzofuran-1(3H)-one (0.95 g, 6.41 mmol), KOH (0.576 g, 10.26 mmol) in methanol (20.52 mL) and water (5.13 mL) was refluxed. After two hr, the reaction was cooled to room temperature, concentrated in vacuo, and acidified with 1 M aqueous KHSO4 to pH ˜3. The mixture was extracted with EtOAc (4×50 mL). The combined extract was dried over MgSO4 and concentrated in vacuo to give the desired product (0.632 g, 3.81 mmol, 59.4% yield) as a white solid.

후처리

  1. concentrationconcentrated in vacuo
  2. extractionThe mixture was extracted with EtOAc (4×50 mL)
  3. extractionThe combined extract
  4. dry with materialwas dried over MgSO4
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-8707a0efd23f4914ba4fe44be75131be
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08685969B2

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