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

HRID 846601

반응식

HRID 846601 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 the ester (2.75 g, 0.0106 mole) 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 solid soon precipitated, and this was filtered, washed with water, air dried, and recrystallized from ethyl acetate (2 crops) to afford 2.03 g (78%) of the title compound as 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. customA solid soon precipitated
  5. filtrationthis was filtered
  6. washwashed with water, air
  7. customdried
  8. customrecrystallized from ethyl acetate (2 crops)

출처 및 근거

ORD 기록
ord-883d96e6799b4a57ada5dddcba134dae
출처 데이터셋
uspto-grants-1992_08
특허 번호
US05137895

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