Water → HCID 66834455, 화합물

HRID 2275133

반응식

HRID 2275133 반응식
[CH2:1]([N:3]([CH2:29][CH3:30])[CH2:4][CH2:5][S:6][C:7]1[CH:8]=[CH:9][C:10]2[C:22](=[O:23])[C:21]3[C:20]4[C:15](=[CH:16][C:17]([C:24]#[N:25])=[CH:18][CH:19]=4)[NH:14][C:13]=3[C:12]([CH3:27])([CH3:26])[C:11]=2[CH:28]=1)[CH3:2].[OH:31]OS([O-])=O.[K+].[OH2:37]>CO>[CH2:29]([N:3]([CH2:1][CH3:2])[CH2:4][CH2:5][S:6]([C:7]1[CH:8]=[CH:9][C:10]2[C:22](=[O:23])[C:21]3[C:20]4[C:15](=[CH:16][C:17]([C:24]#[N:25])=[CH:18][CH:19]=4)[NH:14][C:13]=3[C:12]([CH3:26])([CH3:27])[C:11]=2[CH:28]=1)(=[O:31])=[O:37])[CH3:30]

참가 물질

5

반응물 3

HCID 962WaterHCID 23707502Potassium hydroxy sulfiteHCID 668339748-(2-Diethylamino-ethylsulfanyl)-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile

생성물 1

HCID 66834455HCID 66834455, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

8-(2-Diethylamino-ethylsulfanyl)-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile (Compound B2-17, 16.8 mg, 0.0402 mmol) was dissolved in methanol (1.5 mL), added with oxone (54.3 mg, 2.2 eq.) which had been dissolved in water (0.5 mL), and then stirred at room temperature for 2 hr. The reaction solution was concentrated, extracted with ethyl acetate, washed with saturated sodium hydrogen carbonate, and dried over magnesium sulfate. The drying agent was removed by filtration and the residues obtained after concentration under reduced pressure were purified by silica gel column chromatography (dichloromethane/methanol) to obtain the target compound (white solid, 5.8 mg, 32%).

후처리

  1. concentrationThe reaction solution was concentrated
  2. extractionextracted with ethyl acetate
  3. washwashed with saturated sodium hydrogen carbonate
  4. dry with materialdried over magnesium sulfate
  5. customThe drying agent was removed by filtration
  6. customthe residues obtained
  7. concentrationafter concentration under reduced pressure
  8. customwere purified by silica gel column chromatography (dichloromethane/methanol)
  9. customto obtain the target compound (white solid, 5.8 mg, 32%)

출처 및 근거

ORD 기록
ord-83e01f0eb8e544b4aa32e1a7f13544fb
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09126931B2

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