Hydrochloric Acid → 2-(3-(2-Chloro-6-methylbenzyloxy)phenyl)acetic acid

HRID 516860ノート

反応式

HRID 516860 の反応式
[Cl:1][C:2]1[CH:21]=[CH:20][CH:19]=[C:18]([CH3:22])[C:3]=1[CH2:4][O:5][C:6]1[CH:7]=[C:8]([CH2:12][C:13]([O:15]CC)=[O:14])[CH:9]=[CH:10][CH:11]=1.[OH-].[Na+].Cl>C(O)C>[Cl:1][C:2]1[CH:21]=[CH:20][CH:19]=[C:18]([CH3:22])[C:3]=1[CH2:4][O:5][C:6]1[CH:7]=[C:8]([CH2:12][C:13]([OH:15])=[O:14])[CH:9]=[CH:10][CH:11]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 66875155Ethyl 2-(3-(2-chloro-6-methylbenzyloxy)phenyl)acetate

生成物 1

HCID 445474582-(3-(2-Chloro-6-methylbenzyloxy)phenyl)acetic acid

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a stirred solution of Ethyl 2-(3-(2-chloro-6-methylbenzyloxy)phenyl)acetate (Step B, 4.94 g, 15.5 mmol) in absolute ethanol (80 ml) was added 1N NaOH (40 ml) at room temperature. The reaction mixture was stirred for 3 hours, acidified to pH 3.5-4.0 by adding 1N HCl and concentrated. The residue was taken into chloroform and washed with 0.1N HCl, brine, dried over Na2SO4, filtered, concentrated and purified by flash chromatography on a silica gel column (chloroform:methanol, 95:5 spiked with acetic acid) to give the title compound.

後処理

  1. concentrationconcentrated
  2. washwashed with 0.1N HCl, brine
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. custompurified by flash chromatography on a silica gel column (chloroform:methanol, 95:5 spiked with acetic acid)

出典と根拠

ORDレコード
ord-049cb86012424a4cbfeba75d78999a23
出典データセット
uspto-grants-2015_08
特許番号
US09115072B2

反応ノート

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