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Hydrochloric Acid → 5-(9-Carboxy-nonyloxy)-isophthalic Acid Di-tert-butyl Ester

HRID 1022417
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HRID 1022417 반응식
[C:1]([O:5][C:6](=[O:34])[C:7]1[CH:19]=[C:18]([O:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][C:30]([O:32]C)=[O:31])[CH:17]=[C:9]([C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])[CH:8]=1)([CH3:4])([CH3:3])[CH3:2].[OH-].[Na+].CCOC(C)=O.Cl>C1COCC1>[C:1]([O:5][C:6](=[O:34])[C:7]1[CH:19]=[C:18]([O:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][C:30]([OH:32])=[O:31])[CH:17]=[C:9]([C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])[CH:8]=1)([CH3:2])([CH3:3])[CH3:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 14798Sodium HydroxideHCID 684414955-(9-Methoxycarbonyl-nonyloxy)-isophthalic Acid Di-tert-butyl Ester

생성물 1

HCID 684432455-(9-Carboxy-nonyloxy)-isophthalic Acid Di-tert-butyl Ester

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매

실험 절차

To a solution of 5-(9-methoxycarbonyl-nonyloxy)-isophthalic acid di-tert-butyl ester (162 mg, 0.34 mmol) in THF (2 ml) was added 1 N NaOH (0.35 ml). The mixture was refluxed for 7 h. The mixture was left at room temperature over night before concentration. To the residue EtOAc and 0.1N HCl was added. The aqueous layer was extracted twice with EtOAc. The combined organic layers were washed with brine, dried (Na2SO4) and concentrated to give a clear syrup.

후처리

  1. temperatureThe mixture was refluxed for 7 h
  2. waitThe mixture was left at room temperature over night before concentration
  3. extractionThe aqueous layer was extracted twice with EtOAc
  4. washThe combined organic layers were washed with brine
  5. dry with materialdried (Na2SO4)
  6. concentrationconcentrated
  7. customto give a clear syrup

출처 및 근거

ORD 기록
ord-b19fc40af234415eaf4c55837b010900
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08722620B2

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