Water → 3-(Carboxymethyl)-2-chlorobenzoic acid

HRID 471183ノート

反応式

HRID 471183 の反応式
[OH-:1].[K+].[Cl:3][C:4]1[C:12]([CH2:13][C:14]#N)=[CH:11][CH:10]=[CH:9][C:5]=1[C:6]([OH:8])=[O:7].[OH2:16]>C(O)C>[C:14]([CH2:13][C:12]1[C:4]([Cl:3])=[C:5]([CH:9]=[CH:10][CH:11]=1)[C:6]([OH:8])=[O:7])([OH:16])=[O:1]

参加物

5

反応物 3

HCID 962WaterHCID 14797Potassium HydroxideHCID 579893812-Chloro-3-(cyanomethyl)benzoic acid

生成物 1

HCID 579889673-(Carboxymethyl)-2-chlorobenzoic acid

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Potassium hydroxide (2.976 g) in water (30 mL) was added to a suspension of 2-chloro-3-(cyanomethyl)benzoic acid (example 80, step a) (4.12 g) in ethanol (30 mL) and the resulting solution was heated at reflux for 2 hours, then allowed to cool overnight. The mixture was concentrated in vacuo to remove the ethanol and then diluted with water and washed twice with ethyl acetate. The organic phases were discarded, whilst the aqueous phase was acidified to pH 1 with concentrated hydrochloric acid and extracted three times with ethyl acetate. The combined extracts were dried over anhydrous magnesium sulphate and concentrated in vacuo to afford the crude subtitled compound as a yellow solid. Yield 4.11 g. Used directly.

後処理

  1. temperaturethe resulting solution was heated
  2. temperatureat reflux for 2 hours
  3. temperatureto cool overnight
  4. concentrationThe mixture was concentrated in vacuo
  5. customto remove the ethanol
  6. additiondiluted with water
  7. washwashed twice with ethyl acetate
  8. extractionextracted three times with ethyl acetate
  9. dry with materialThe combined extracts were dried over anhydrous magnesium sulphate
  10. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-7e233b89c462424286ea314c5e86fab2
出典データセット
uspto-grants-2014_01
特許番号
US08629271B2

反応ノート

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