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Sodium Bicarbonate → 12-Chloro-6,6-dioxo-5,6-dihydro-6lambda*6*-thia-4,5-diaza-chrysen-9-ylamine

HRID 513773
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HRID 513773 반응식
C([NH:8][C:9]1[CH:26]=[C:25]2[C:12]([S:13](=[O:29])(=[O:28])[NH:14][C:15]3[C:24]2=[CH:23][C:22]([Cl:27])=[C:21]2[C:16]=3[N:17]=[CH:18][CH:19]=[CH:20]2)=[CH:11][CH:10]=1)C1C=CC=CC=1.C([O-])(O)=O.[Na+]>Br>[Cl:27][C:22]1[CH:23]=[C:24]2[C:15](=[C:16]3[C:21]=1[CH:20]=[CH:19][CH:18]=[N:17]3)[NH:14][S:13](=[O:28])(=[O:29])[C:12]1[C:25]2=[CH:26][C:9]([NH2:8])=[CH:10][CH:11]=1
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참가 물질

4

반응물 2

HCID 516892Sodium BicarbonateHCID 68183316Benzyl-(12-chloro-6,6-dioxo-5,6-dihydro-6lambda*6*-thia-4,5-diaza-chrysen-9-yl)-amine

생성물 1

HCID 6819028412-Chloro-6,6-dioxo-5,6-dihydro-6lambda*6*-thia-4,5-diaza-chrysen-9-ylamine수율 77%

시약·촉매·용매 1

HCID 260Hydrogen Bromide용매

실험 절차

A solution of benzyl-(12-chloro-6,6-dioxo-5,6-dihydro-6λ*6*-thia-4,5-diaza-chrysen-9-yl)-amine 513 (218 mg, 0.52 mmol) in 48% aq. HBr (5 ml) was heated at 100° C. in a sealed tube for 3 h. After cooling, the mixture was neutralized with sat. NaHCO3 solution and the aqueous phase was extracted with EtOAc. The organic phase was washed with water, brine, dried (Na2SO4) and concentrated in vacuo. The crude residue was purified by column chromatography with DCM as the eluent to give the title compound (50 mg, 77%).

후처리

  1. temperatureAfter cooling
  2. extractionthe aqueous phase was extracted with EtOAc
  3. washThe organic phase was washed with water, brine
  4. dry with materialdried (Na2SO4)
  5. concentrationconcentrated in vacuo
  6. customThe crude residue was purified by column chromatography with DCM as the eluent

출처 및 근거

ORD 기록
ord-c25b1f9893444ecf92774f3f2429ff50
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09102688B2

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