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Hydrochloric Acid → HCID 15439079、化合物

HRID 1365024
ノート
印刷プレビュー

反応式

HRID 1365024 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

HCID 15439079HCID 15439079、化合物収率 80.1%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-d343882b5c104b7197b19e8363d0db78
出典データセット
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07888487B2

反応ノート

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