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Acetone → HCID 12940140、化合物

HRID 848060
ノート
印刷プレビュー

反応式

HRID 848060 の反応式
[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
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 180AcetoneHCID 7969ThiophenolHCID 14798Sodium HydroxideHCID 129224872-[(1,2,2,2-Tetrachloroethyl)carbamoyl]phenyl acetate

生成物 1

HCID 12940140HCID 12940140、化合物収率 80%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-aca51e34939148f48da36d6deadfc7f0
出典データセット
uspto-grants-1981_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04294835

反応ノート

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