Hydrochloric Acid → 4-Cyanoisophthalic acid

HRID 2414222ノート

反応式

HRID 2414222 の反応式
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]

参加物

6

反応物 3

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

生成物 1

HCID 226444314-Cyanoisophthalic acid

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-677ec35014b0470caa8a41ef9c3e3026
出典データセット
uspto-grants-2004_11
特許番号
US06811979B2

反応ノート

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