Hydrochloric Acid → 4-(2-Methoxyethoxymethoxy)benzoic acid

HRID 1777275ノート

反応式

HRID 1777275 の反応式
[OH-].[Na+].[CH3:3][O:4][CH2:5][CH2:6][O:7][CH2:8][O:9][C:10]1[CH:19]=[CH:18][C:13]([C:14]([O:16]C)=[O:15])=[CH:12][CH:11]=1.Cl>O1CCCC1.O.CO.C(OCC)(=O)C>[CH3:3][O:4][CH2:5][CH2:6][O:7][CH2:8][O:9][C:10]1[CH:19]=[CH:18][C:13]([C:14]([OH:16])=[O:15])=[CH:12][CH:11]=1

参加物

8

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 67056306Methyl 4-(2-methoxyethoxymethoxy)benzoate

生成物 1

HCID 149522434-(2-Methoxyethoxymethoxy)benzoic acid収率 95%

試薬・触媒・溶媒 4

HCID 887Methanol溶媒HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
40 °C

実験手順

15 g (375 mmol) of sodium hydroxide powder are added to a solution of 16 g (75 mmol) of methyl 4-(2-methoxyethoxymethoxy)benzoate in 250 ml of tetrahydrofuran, 80 ml of water and 30 ml of methanol. The reaction medium is stirred at 40° C. for 18 h then hydrolysed, diluted with ethyl acetate and brought to pH=6 with an aqueous solution of hydrochloric acid having a concentration of 1N. After extracting with ethyl acetate, the organic phase is washed with water then with a saturated aqueous solution of sodium chloride, dried over magnesium sulphate, filtered then concentrated. 16 g (95%) of 4-(2-methoxyethoxymethoxy)benzoic acid are obtained in the form of a white solid.

後処理

  1. extractionAfter extracting with ethyl acetate
  2. washthe organic phase is washed with water
  3. dry with materialwith a saturated aqueous solution of sodium chloride, dried over magnesium sulphate
  4. filtrationfiltered
  5. concentrationthen concentrated

出典と根拠

ORDレコード
ord-d0bb91093c1a4c6cb09c6dbec7824b6f
出典データセット
uspto-grants-2016_02
特許番号
US09266848B2

反応ノート

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