2-Chloro-3',4'-dihydroxyacetophenone → HCID 178515889, 화합물

HRID 483361

반응식

HRID 483361 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

HCID 178515889HCID 178515889, 화합물수율 72.9%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2415b5230c51422e806ffa8b944759b4
출처 데이터셋
uspto-grants-1993_07
특허 번호
US05225406

연결된 노트

불러오는 중…