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Hydrochloric Acid → HCID 15439079, 화합물

HRID 1365024
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HRID 1365024 반응식
[NH2-].[Na+].CS[C:5](=[S:14])[O:6][CH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[CH3:15][O:16][C:17]1[CH:30]=[CH:29][C:20]([C:21]([C:23]2C=CC=CC=2)=[O:22])=[CH:19][CH:18]=1.Cl>C1(C)C=CC=CC=1>[CH2:7]([O:6][C:5](=[S:14])[CH2:23][C:21]([C:20]1[CH:29]=[CH:30][C:17]([O:16][CH3:15])=[CH:18][CH:19]=1)=[O:22])[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 24533Sodium amideHCID 691464-MethoxybenzophenoneHCID 3415526O-Benzyl S-methyl dithiocarbonate

생성물 1

HCID 15439079HCID 15439079, 화합물수율 80.1%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

To a suspension of sodium amide (1.6 g) in toluene (50 mL) was added a mixture of dithiocarbonic acid O-benzyl ester S-methyl ester (4.0 g) and 4-methoxybenzophenone (3.0 g) at room temperature and the mixture was stirred at room temperature overnight. Hydrochloric acid solution (2 mol/L, 80 mL) was added to the reaction mixture and the mixture was extracted with diethyl ether. The organic layer was washed with brine and dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure. The residue was purified by column chromatography on silica gel (eluent: hexane/dichloromethane=5/1-2/1) to give the title compound (3.4 g).

후처리

  1. additionwas added
  2. extractionthe mixture was extracted with diethyl ether
  3. washThe organic layer was washed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customthe solvent was removed under reduced pressure
  6. customThe residue was purified by column chromatography on silica gel (eluent: hexane/dichloromethane=5/1-2/1)

출처 및 근거

ORD 기록
ord-d343882b5c104b7197b19e8363d0db78
출처 데이터셋
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07888487B2

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