Hydrochloric Acid → HCID 67401877, 화합물

HRID 906109노트

반응식

HRID 906109 반응식
[OH:1][CH2:2][CH2:3][C:4]#[C:5][C:6]1[C:15]([O:16][CH3:17])=[CH:14][CH:13]=[CH:12][C:7]=1[C:8]([O:10]C)=[O:9].[OH-].[K+].Cl>CO.O>[OH:1][CH2:2][CH2:3][C:4]#[C:5][C:6]1[C:15]([O:16][CH3:17])=[CH:14][CH:13]=[CH:12][C:7]=1[C:8]([OH:10])=[O:9]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 67402660HCID 67402660, 화합물

생성물 1

HCID 67401877HCID 67401877, 화합물수율 99%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

반응 조건

온도
60 °C

실험 절차

Methyl 2-(4-hydroxybut-1-yn-1-yl)-3-(methyloxy)benzoate (0.056 g, 0.24 mmol) was dissolved in methanol (2 ml), and a solution of potassium hydroxide (0.027 g, 0.48 mmol) in water (0.5 ml) was added. The reaction mixture was stirred at 60° C. for 1 h, cooled to room temperature, and 1.5M hydrochloric acid was added to pH 4. The aqueous mixture was extracted with ethyl acetate, and the organic layer was washed with brine then dried over sodium sulfate. The mixture was then filtered and concentrated to give 2-(4-hydroxybut-1-yn-1-yl)-3-(methyloxy)benzoic acid (0.052 g, 99% yield). MS (EI) for C12H12O4: 219 (M−H).

후처리

  1. temperaturecooled to room temperature
  2. extractionThe aqueous mixture was extracted with ethyl acetate
  3. washthe organic layer was washed with brine
  4. dry with materialthen dried over sodium sulfate
  5. filtrationThe mixture was then filtered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-63d9d8e13718418fadf74cf281a8491b
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08012956B2

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