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Hydrochloric Acid → 3-(5-Phenyl-3-isoxazolyl)benzoic acid

HRID 1354436
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HRID 1354436 반응식
[C:1]1([C:7]2[O:11][N:10]=[C:9]([C:12]3[CH:13]=[C:14]([CH:19]=[CH:20][CH:21]=3)[C:15]([O:17]C)=[O:16])[CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[OH-].[Na+].O1CCCC1.Cl>O.CO>[C:1]1([C:7]2[O:11][N:10]=[C:9]([C:12]3[CH:13]=[C:14]([CH:19]=[CH:20][CH:21]=3)[C:15]([OH:17])=[O:16])[CH:8]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 22934547Methyl 3-(5-phenyl-3-isoxazolyl)benzoate

생성물 1

HCID 229345643-(5-Phenyl-3-isoxazolyl)benzoic acid수율 85%

시약·촉매·용매 2

HCID 887Methanol용매
HCID 962Water용매

반응 조건

온도
60 °C

실험 절차

A mixture of methyl 3-(5-phenyl-3-isoxazolyl)benzoate (1.30 g), 1 M aqueous sodium hydroxide solution (10 ml), tetrahydrofuran (20 ml) and methanol (10 ml) was stirred at 60° C. for 1 hr. After cooling, the reaction mixture was poured into water, and 1 M hydrochloric acid (10 ml) was added. The crystals were collected by filtration and recrystallized from tetrahydrofuran-hexane to give 3-(5-phenyl-3-isoxazolyl)benzoic acid (1.05 g, yield 85%) as colorless crystals. melting point: 250–251° C.

후처리

  1. temperatureAfter cooling
  2. additionwas added
  3. filtrationThe crystals were collected by filtration
  4. customrecrystallized from tetrahydrofuran-hexane

출처 및 근거

ORD 기록
ord-551a8fde9d2a46e481410d481f2261ac
출처 데이터셋
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07223791B2

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