Hydrochloric Acid → 4-{3-Cyano-4-[2-(2-methoxyethoxy)phenyl]pyrrole-1-yl}-2-hydroxy benzoic acid

HRID 570843노트

반응식

HRID 570843 반응식
C([O:3][C:4](=[O:30])[C:5]1[CH:10]=[CH:9][C:8]([N:11]2[CH:15]=[C:14]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[O:22][CH2:23][CH2:24][O:25][CH3:26])[C:13]([C:27]#[N:28])=[CH:12]2)=[CH:7][C:6]=1[OH:29])C.C(O)C.[OH-].[Li+].Cl>O.O1CCCC1>[C:27]([C:13]1[C:14]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[O:22][CH2:23][CH2:24][O:25][CH3:26])=[CH:15][N:11]([C:8]2[CH:9]=[CH:10][C:5]([C:4]([OH:30])=[O:3])=[C:6]([OH:29])[CH:7]=2)[CH:12]=1)#[N:28]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 3939Lithium HydroxideHCID 685064744-{3-Cyano-4-[2-(2-methoxyethoxy)phenyl]pyrrole-1-yl}-2-hydroxy benzoic acid ethyl ester

생성물 1

HCID 250521924-{3-Cyano-4-[2-(2-methoxyethoxy)phenyl]pyrrole-1-yl}-2-hydroxy benzoic acid수율 76.1%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 4-{3-cyano-4-[2-(2-methoxyethoxy)phenyl]pyrrole-1-yl}-2-hydroxy benzoic acid ethyl ester (0.072 g) in a mixed solvent of ethanol (9 mL) and tetrahydrofuran (3 mL) was added 1 mol/mL aqueous lithium hydroxide solution (2.7 mL), and this mixture was stirred at room temperature for 48 hours. This reaction mixture was poured into 1 mol/L hydrochloric acid (2.7 mL), and to this mixture was added water (30 mL). The precipitated solid was collected by filtration. This obtained solid was washed with water, dried under reduced pressure at 50° C. to give the title compound (0.051 g).

후처리

  1. filtrationThe precipitated solid was collected by filtration
  2. washThis obtained solid was washed with water
  3. customdried under reduced pressure at 50° C.

출처 및 근거

ORD 기록
ord-a54a1c8fc3bb46fca5466b1a9772f379
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09023882B2

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