2-Chloro-3',4'-dihydroxyacetophenone → HCID 178515889、化合物

HRID 483361

反応式

HRID 483361 の反応式
Cl[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([OH:11])=[C:7]([OH:12])[CH:6]=1)=O.[C:13](=[S:16])([S-:15])[NH2:14].[NH4+]>CO>[OH:12][C:7]1[CH:6]=[C:5]([C:3]2[N:14]=[C:13]([SH:16])[S:15][CH:2]=2)[CH:10]=[CH:9][C:8]=1[OH:11]

参加物

4

反応物 2

HCID 668342-Chloro-3',4'-dihydroxyacetophenoneHCID 11083854Ammonium dithiocarbamate

生成物 1

HCID 178515889HCID 178515889、化合物収率 72.9%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

10.0 g (53.6 mmol) of 2-chloro-3'4'-dihydroxyacetophenone was dissolved in 100 ml of methanol, and then 5.90 g (53.6 mmol) of ammonium dithiocarbamate was added thereto. The mixture was stirred at room temperature for 30 minutes. The solvent was distilled off under reduced pressure. To the residue, water was added to adjust the mixture to pH2.0, and then the mixture was extracted twice with ethyl acetate. The extract was dried over anhydrous sodium sulfate and-then concentrated. The crystal residue was washed with diethyl ether to obtain 8.80 g (yield: 72.9%) of the above-identified compound.

後処理

  1. distillationThe solvent was distilled off under reduced pressure
  2. additionTo the residue, water was added
  3. extractionthe mixture was extracted twice with ethyl acetate
  4. dry with materialThe extract was dried over anhydrous sodium sulfate
  5. concentrationconcentrated
  6. washThe crystal residue was washed with diethyl ether

出典と根拠

ORDレコード
ord-2415b5230c51422e806ffa8b944759b4
出典データセット
uspto-grants-1993_07
特許番号
US05225406

関連ノート

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