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Acetone → HCID 12940140, 화합물

HRID 848060
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HRID 848060 반응식
[OH-].[Na+].Cl[CH:4]([NH:9][C:10](=[O:21])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[O:17]C(=O)C)[C:5]([Cl:8])([Cl:7])[Cl:6].CC(C)=O.[C:26]1([SH:32])[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1>O>[C:26]1([S:32][CH:4]([NH:9][C:10](=[O:21])[C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[OH:17])[C:5]([Cl:6])([Cl:7])[Cl:8])[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 180AcetoneHCID 7969ThiophenolHCID 14798Sodium HydroxideHCID 129224872-[(1,2,2,2-Tetrachloroethyl)carbamoyl]phenyl acetate

생성물 1

HCID 12940140HCID 12940140, 화합물수율 80%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

10.3 g of a 20% acqueous NaOH solution was added dropwise to the mixture of 16.6 g of N-(1,2,2,2-tetrachloroethyl)-2-acetoxybenzamide, 70 ml of acetone and 5.3 g of phenyl mercaptan under stirring at 10°-15° C. The reaction was effected at room temperature for one hour. Water was added thereto, the dichloromethane layer was separated, and the solution was dried and concentrated. 100 ml of ethanol and 1.5 ml of 35% hydrochloric acid were added to the residue and the reaction was effected under reflux for two hours. The solvent was distilled off to obtain 14.5 g of N-(1-phenylthio-2,2,2-trichloroethyl)-2-hydroxybenzamide as white crystals.

후처리

  1. customthe dichloromethane layer was separated
  2. customthe solution was dried
  3. concentrationconcentrated
  4. addition100 ml of ethanol and 1.5 ml of 35% hydrochloric acid were added to the residue
  5. temperatureunder reflux for two hours
  6. distillationThe solvent was distilled off

출처 및 근거

ORD 기록
ord-aca51e34939148f48da36d6deadfc7f0
출처 데이터셋
uspto-grants-1981_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04294835

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