Water → 4-Amino-5-chloro-2-(2-methoxyethoxy)benzoic acid

HRID 2254610

반응식

HRID 2254610 반응식
C[O:2][C:3](=[O:17])[C:4]1[CH:9]=[C:8]([Cl:10])[C:7]([NH2:11])=[CH:6][C:5]=1[O:12][CH2:13][CH2:14][O:15][CH3:16].[OH-].[Na+].O>C(O)C>[NH2:11][C:7]1[C:8]([Cl:10])=[CH:9][C:4]([C:3]([OH:17])=[O:2])=[C:5]([O:12][CH2:13][CH2:14][O:15][CH3:16])[CH:6]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 539320764-Amino-5-chloro-2-(2-methoxyethoxy)benzoic acid methyl ester

생성물 1

HCID 197959774-Amino-5-chloro-2-(2-methoxyethoxy)benzoic acid수율 78%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 4-amino-5-chloro-2-(2-methoxyethoxy)benzoic acid methyl ester (2.75 g, 10.6 mmoles) in 95% ethanol (20 ml) was treated with 50% sodium hydroxide (10 ml) and water (10 ml), and refluxed for one hour. The ethanol was removed in vacuo and replaced with water, and the aqueous solution was extracted with ether (20 ml) and adjusted to pH 4 with concentrated hydrochloric acid (16 ml). A resultant precipitate was filtered, washed with water, air dried, and recrystallized from ethyl acetate to yield 2.03 g (78%) of fine pale tan needles, mp 119°-120° C.

후처리

  1. temperaturerefluxed for one hour
  2. customThe ethanol was removed in vacuo
  3. extractionthe aqueous solution was extracted with ether (20 ml)
  4. filtrationA resultant precipitate was filtered
  5. washwashed with water, air
  6. customdried
  7. customrecrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-02a4994f0c0241dc84fc7c631bbbac03
출처 데이터셋
uspto-grants-1993_08
특허 번호
US05236931

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