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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
ノート
印刷プレビュー

反応式

HRID 513773 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 260Hydrogen Bromide溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-c25b1f9893444ecf92774f3f2429ff50
出典データセット
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09102688B2

反応ノート

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