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Hydrochloric Acid → 4-Amino-5,6-dichloropicolinic Acid

HRID 2407809
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HRID 2407809 반응식
[NH2:1][C:2]1[C:7]([Cl:8])=[C:6]([Cl:9])[N:5]=[C:4]([C:10]([O:12]C)=[O:11])[CH:3]=1.C[Si](C)(C)[O-].[K+].Cl.C(OCC)(=O)C>O1CCCC1.O>[NH2:1][C:2]1[C:7]([Cl:8])=[C:6]([Cl:9])[N:5]=[C:4]([C:10]([OH:12])=[O:11])[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 23668039Potassium trimethylsilanolateHCID 58504072Methyl 4-amino-5,6-dichloro-2-pyridinecarboxylate

생성물 1

HCID 585040704-Amino-5,6-dichloropicolinic Acid수율 98.5%

시약·촉매·용매 2

HCID 962Water용매

실험 절차

The compound prepared in Example 405 (2.438 g) and potassium trimethylsilanolate (2.971 g) were suspended in tetrahydrofuran (100 mL) and stirred at reflux for 4 hours. The reaction mixture was dissolved in water and added to 1 N hydrochloric acid. Ethyl acetate was added and the system stirred at room temperature. The organics were dried, magnesium sulfate and concentrated under reduced pressure to furnish the title compound (2.250 g), which was used without further purification, possessing the following physical data.

후처리

  1. temperatureat reflux for 4 hours
  2. stirringthe system stirred at room temperature
  3. customThe organics were dried
  4. concentrationmagnesium sulfate and concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-2d3e1c67be8e44c29e6804966f15762b
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08809538B2

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이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트
HCID 8028
Tetrahydrofuran
용매