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

HRID 516860노트

반응식

HRID 516860 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-049cb86012424a4cbfeba75d78999a23
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09115072B2

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