Hydrochloric Acid → HCID 67401877、化合物

HRID 906109ノート

反応式

HRID 906109 の反応式
[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]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 67402660HCID 67402660、化合物

生成物 1

HCID 67401877HCID 67401877、化合物収率 99%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

反応条件

温度
60 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-63d9d8e13718418fadf74cf281a8491b
出典データセット
uspto-grants-2011_09
特許番号
US08012956B2

反応ノート

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