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Hydrochloric Acid → 4-Ethoxy-2,3-difluoro-4'-biphenylbenzoic acid

HRID 1943556
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HRID 1943556 반응식
[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[CH:15]=[CH:14][C:13]([C:16]3[C:21]([C:22]([O:24]CC)=[O:23])=[CH:20][CH:19]=[CH:18][CH:17]=3)=[CH:12][CH:11]=2)=[C:6]([F:27])[C:5]=1[F:28])[CH3:2].[OH-].[Na+].O.Cl>C1(C)C=CC=CC=1>[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[CH:11]=[CH:12][C:13]([C:16]3[C:21]([C:22]([OH:24])=[O:23])=[CH:20][CH:19]=[CH:18][CH:17]=3)=[CH:14][CH:15]=2)=[C:6]([F:27])[C:5]=1[F:28])[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 14798Sodium HydroxideHCID 66682456Ethyl 4-ethoxy-2,3-difluoro-4'-biphenylbenzoate

생성물 1

HCID 670823704-Ethoxy-2,3-difluoro-4'-biphenylbenzoic acid수율 48.2%

시약·촉매·용매 1

HCID 1140Toluene
용매

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온도
30 °C

실험 절차

The compounds (3) (29.1 g), sodium hydroxide (11.4 g), Solmix A-11 (100 ml) and water (100 ml) were mixed, and the mixture was heated under reflux for 2 hours. The reaction mixture was cooled to 30° C., and then aqueous 6N-hydrochloric acid solution (100 ml) and toluene (200 ml) were added hereto and mixed. The mixture was then allowed to stand until it had separated into two phases of organic and aqueous phases, and extraction into an organic phase was carried out. The organic phase obtained was fractionated, washed sequentially with water, a saturated aqueous solution of sodium hydrogencarbonate and water, and then dried over anhydrous magnesium sulfate, giving 13.0 g of 4-ethoxy-2,3-difluoro-4′-biphenylbenzoic acid (44). The yield based on the compound (3) was 49.2%.

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 2 hours
  3. additionmixed
  4. customhad separated into two phases of organic and
  5. extractionaqueous phases, and extraction into an organic phase
  6. customThe organic phase obtained
  7. washwashed sequentially with water
  8. dry with materiala saturated aqueous solution of sodium hydrogencarbonate and water, and then dried over anhydrous magnesium sulfate

출처 및 근거

ORD 기록
ord-5480e426a06b488cae572174ad93f673
출처 데이터셋
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08394294B2

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