Hydrochloric Acid → 4-Cyanoisophthalic acid

HRID 2414222노트

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HRID 2414222 반응식
C[O:2][C:3](=[O:16])[C:4]1[CH:13]=[CH:12][C:11]([C:14]#[N:15])=[C:6]([C:7]([O:9]C)=[O:8])[CH:5]=1.[OH-].[Li+].Cl>CO.O>[C:14]([C:11]1[CH:12]=[CH:13][C:4]([C:3]([OH:16])=[O:2])=[CH:5][C:6]=1[C:7]([OH:9])=[O:8])#[N:15]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 10376118Dimethyl 4-cyano-1,3-benzenedicarboxylate

생성물 1

HCID 226444314-Cyanoisophthalic acid

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

4-Cyanoisophthalic acid dimethyl ester 203 (1.70 g, 7.76 mmol) was dissolved in methanol (100 mL) and then treated with an aqueous solution of lithium hydroxide (2.0 g, 46.5 mmol) in 50 mL of water. The basic solution was stirred at ambient temperature for 1.5 hour. It was then poured into a 10% HCl solution. The solution was extracted with ethyl acetate and the combined extracts were dried over Na2SO4. Removal of solvent gave quantitative yield of 4-cyanoisophthalic acid 204: 1H NMR (400 MHz, CD3OD) δ 8.01 (d, J=8 Hz, 1H), 8.33 (dd, J=1.7 Hz, J=8 Hz, 1H), 8.73 (d, J=1.7 Hz, 1H).

후처리

  1. extractionThe solution was extracted with ethyl acetate
  2. dry with materialthe combined extracts were dried over Na2SO4
  3. customRemoval of solvent

출처 및 근거

ORD 기록
ord-677ec35014b0470caa8a41ef9c3e3026
출처 데이터셋
uspto-grants-2004_11
특허 번호
US06811979B2

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