Potassium Carbonate → HCID 46232618, 화합물

HRID 83108

반응식

HRID 83108 반응식
[OH:1][C:2]1[C:15]2[C:14](=[O:16])[C:13]3[CH:12]=[C:11]4[CH:17]=[CH:18][CH:19]=[CH:20][C:10]4=[CH:9][C:8]=3[O:7][C:6]=2[CH:5]=[C:4]([OH:21])[CH:3]=1.C([O-])([O-])=O.[K+].[K+].[CH2:28]1[S:30][CH:29]1[CH2:31]Cl>CC(C)=O>[OH:1][C:2]1[C:15]2[C:14](=[O:16])[C:13]3[CH:12]=[C:11]4[CH:17]=[CH:18][CH:19]=[CH:20][C:10]4=[CH:9][C:8]=3[O:7][C:6]=2[CH:5]=[C:4]([O:21][CH2:31][CH:29]2[CH2:28][S:30]2)[CH:3]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 18588EpithiochlorohydrinHCID 107077051,3-dihydroxy-12H-benzo(b)xanthen-12-one

생성물 1

HCID 46232618HCID 46232618, 화합물수율 20.8%

시약·촉매·용매 1

HCID 180Acetone용매2회

반응 조건

온도
57.5 °C

실험 절차

1,3-dihydroxy-12H-benzo[b]xanthen-12-one (0.05 g, 0.18 mmol) synthesized in Step 1 of Example 18, K2CO3 (0.07 g, 0.54 mmol), and anhydrous acetone (18 mL) were charged to a dry round-bottom flask. Under stirring, epithiochlorohydrin (0.07 g, 0.72 mmol) dissolved in anhydrous acetone (2 mL) was added thereto. The reaction liquid was stirred with reflux at a temperature of 55 to 60° C. under a nitrogen atmosphere (overnight). Solid of the reaction mixture was filtered and removed, and the filtrate was concentrated under reduced pressure. The resulting residue was separated and purified by silica gel column chromatography (developing solvent: ethyl acetate:n-hexane=1:3 (v/v)) to give the title compound (13.1 mg, 20.8%) as a yellow solid.

후처리

  1. additionwas added
  2. customThe reaction liquid
  3. stirringwas stirred
  4. filtrationSolid of the reaction mixture was filtered
  5. customremoved
  6. concentrationthe filtrate was concentrated under reduced pressure
  7. customThe resulting residue was separated
  8. custompurified by silica gel column chromatography (developing solvent: ethyl acetate:n-hexane=1:3 (v/v))

출처 및 근거

ORD 기록
ord-847200c51ac644d7879d0a32c9faa962
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846749B2

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