Hydrochloric Acid → 2-[7-Bromo-3-(4-bromo-2-fluorobenzyl)-1,2,3,4-tetrahydro-2,4-dioxoquinazolin-1-yl]acetic acid

HRID 569828

반응식

HRID 569828 반응식
[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6](=[O:28])[N:7]([CH2:19][C:20]3[CH:25]=[CH:24][C:23]([Br:26])=[CH:22][C:21]=3[F:27])[C:8](=[O:18])[N:9]2[CH2:12][C:13]([O:15]CC)=[O:14])=[CH:4][CH:3]=1.[OH-].[Na+].Cl>CO>[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6](=[O:28])[N:7]([CH2:19][C:20]3[CH:25]=[CH:24][C:23]([Br:26])=[CH:22][C:21]=3[F:27])[C:8](=[O:18])[N:9]2[CH2:12][C:13]([OH:15])=[O:14])=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 14458963Ethyl 2-[7-bromo-3-(4-bromo-2-fluorobenzyl)-1,2,3,4-tetrahydro-2,4-dioxoquinazolin-1-yl]acetate

생성물 1

HCID 144238012-[7-Bromo-3-(4-bromo-2-fluorobenzyl)-1,2,3,4-tetrahydro-2,4-dioxoquinazolin-1-yl]acetic acid수율 83.2%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of ethyl 2-[7-bromo-3-(4-bromo-2-fluorobenzyl)-1,2,3,4-tetrahydro-2,4-dioxoquinazolin-1-yl]acetate (3.0 g) and 1N aqueous sodium hydroxide (5.83 ml) in methanol (69.6 ml) was refluxed for 1 hour with stirring. After cooling, the solvent was evaporated to give a residue, which was acidified with 1N aqueous hydrochloric acid and extracted with ethyl acetate. The extract was washed with brine and dried. Removal of the solvent gave a residue, which was recrystallized from a mixture of ethyl acetate and n-hexane to afford 2-[7-bromo-3-(4-bromo-2-fluorobenzyl)-1,2,3,4-tetrahydro-2,4-dioxoquinazolin-1-yl]acetic acid (2.36 g).

후처리

  1. temperatureAfter cooling
  2. customthe solvent was evaporated
  3. customto give a residue, which
  4. extractionextracted with ethyl acetate
  5. washThe extract was washed with brine
  6. customdried
  7. customRemoval of the solvent
  8. customgave a residue, which
  9. customwas recrystallized from a mixture of ethyl acetate and n-hexane

출처 및 근거

ORD 기록
ord-5935f0a18de34bda938c756ed067768e
출처 데이터셋
uspto-grants-1988_03
특허 번호
US04734419

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