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Hydrochloric Acid → HCID 89767889, 화합물

HRID 591484
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인쇄 미리보기

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HRID 591484 반응식
C([O:5][C:6](=[O:33])[CH2:7][O:8][C:9]1[C:13]2[CH:14]=[CH:15][C:16]([O:18][CH2:19][C:20]3[CH:25]=[CH:24][C:23]([Cl:26])=[CH:22][C:21]=3[Cl:27])=[CH:17][C:12]=2[S:11][C:10]=1[C:28]([O:30]CC)=[O:29])(C)(C)C.[OH-].[Na+].CCO.Cl>O.C1COCC1>[C:6]([CH2:7][O:8][C:9]1[C:13]2[CH:14]=[CH:15][C:16]([O:18][CH2:19][C:20]3[CH:25]=[CH:24][C:23]([Cl:26])=[CH:22][C:21]=3[Cl:27])=[CH:17][C:12]=2[S:11][C:10]=1[C:28]([OH:30])=[O:29])([OH:33])=[O:5]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 14798Sodium HydroxideHCID 89767477HCID 89767477, 화합물

생성물 1

HCID 89767889HCID 89767889, 화합물수율 92.5%

시약·촉매·용매 2

HCID 962Water용매
HCID 8028
Tetrahydrofuran
용매

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온도
50 °C

실험 절차

A mixture of ethyl 3-(2-tert-butoxy-2-oxoethoxy)-6-((2,4-dichlorobenzyl)oxy)-1-benzothiophene-2-carboxylate (1.1 g), 1N NaOH (5 mL), EtOH (5 mL) and THF (10 mL) was stirred at 50° C. for 24 h. Water and 1N HCl (5 mL) were added to the mixture and the mixture was extracted with THF-EtOAc. The organic layer was washed with brine, dried over MgSO4 and concentrated in vacuo. The residue was washed with hexane to give the title compound (0.850 g). The obtained crystals were recrystallized from acetone-water.

후처리

  1. extractionthe mixture was extracted with THF-EtOAc
  2. washThe organic layer was washed with brine
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated in vacuo
  5. washThe residue was washed with hexane

출처 및 근거

ORD 기록
ord-71dcd808ac204434a86f1bb59418d602
출처 데이터셋
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09238639B2

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