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tert-Butanol → Tert-butyl (2-bromo-5,6,7,8-tetrahydroimidazo[1,2-a]pyridin-7-yl)carbamate

HRID 874345
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HRID 874345 반응식
[C:1]([OH:5])([CH3:4])([CH3:3])[CH3:2].[Br:6][C:7]1[N:8]=[C:9]2[CH2:14][CH:13](C(O)=O)[CH2:12][CH2:11][N:10]2[CH:18]=1.[N-:19]=[N+]=[N-].P([O-])([O:31][C:32]1C=CC=CC=1)(OC1C=CC=CC=1)=O>C(N(CC)CC)C>[Br:6][C:7]1[N:8]=[C:9]2[CH2:14][CH:13]([NH:19][C:32](=[O:31])[O:5][C:1]([CH3:4])([CH3:3])[CH3:2])[CH2:12][CH2:11][N:10]2[CH:18]=1
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참가 물질

5

반응물 3

HCID 6386tert-ButanolHCID 21964642Diphenylphosphate azideHCID 903832892-Bromo-5,6,7,8-tetrahydroimidazo[1,2-a]pyridine-7-carboxylic acid

생성물 1

HCID 90383235Tert-butyl (2-bromo-5,6,7,8-tetrahydroimidazo[1,2-a]pyridin-7-yl)carbamate

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

Molecular Sieves 4 A (6 g) was added to a tert-butanol (45 ml) solution of the 2-bromo-5,6,7,8-tetrahydroimidazo[1,2-a]pyridine-7-carboxylic acid (3.1 g) obtained in (Example 2.7) <Step 3> and triethylamine (9.7 ml), and the obtained mixture was then stirred at room temperature for 30 minutes. Thereafter, diphenyl phosphate azide (3.8 ml) was added to the reaction solution, and the obtained mixture was stirred for 30 minutes and then at 110° C. for 4 hours. Thereafter, the reaction solution was filtered with Celite, and insoluble matters were then washed with ethyl acetate. After that, ethyl acetate (100 ml) was added to the filtrate, and the obtained mixture was successively washed with a saturated ammonium chloride aqueous solution (25 ml) three times, a saturated sodium hydrogen carbonate aqueous solution (25 ml) twice, and a saturated saline. Then, the solvent was distilled away under reduced pressure. Methylene chloride was added to the obtained residue, and precipitated white insoluble matters were then removed by suction filtration. The filtrate was concentrated under reduced pressure, and the obtained residue was then purified by silica gel column chromatography (silica gel:eluent; heptane:ethyl acetate=60:40-20:80), so as to obtain the title compound (1.3 g) in the form of a white solid.

후처리

  1. stirringthe obtained mixture was stirred for 30 minutes
  2. waitat 110° C. for 4 hours
  3. filtrationThereafter, the reaction solution was filtered with Celite, and insoluble matters
  4. washwere then washed with ethyl acetate
  5. additionAfter that, ethyl acetate (100 ml) was added to the filtrate
  6. washthe obtained mixture was successively washed with a saturated ammonium chloride aqueous solution (25 ml) three times
  7. distillationThen, the solvent was distilled away under reduced pressure
  8. additionMethylene chloride was added to the obtained residue
  9. customprecipitated white insoluble matters
  10. customwere then removed by suction filtration
  11. concentrationThe filtrate was concentrated under reduced pressure
  12. customthe obtained residue was then purified by silica gel column chromatography (silica gel:eluent; heptane:ethyl acetate=60:40-20:80)

출처 및 근거

ORD 기록
ord-4f37af0b10734a3e837964cccecd840a
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08980888B2

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