Hydrochloric Acid → Ethyl 4-isothiocyanatobenzoate
反応式
[NH2:1][C:2]1[CH:12]=[CH:11][C:5]([C:6]([O:8][CH2:9][CH3:10])=[O:7])=[CH:4][CH:3]=1.C(N(CC)[C:16](Cl)=[S:17])C.Cl>C1(C)C=CC=CC=1>[N:1]([C:2]1[CH:3]=[CH:4][C:5]([C:6]([O:8][CH2:9][CH3:10])=[O:7])=[CH:11][CH:12]=1)=[C:16]=[S:17]参加物
5
実験手順
82.5 g of ethyl p-aminobenzoate was dissolved in 500 ml of toluene, to the solution was added 83.4 g of N,N-diethylthiocarbamoyl chloride and the mixture was refluxed by heating for 8 hours. After cooling with ice, 100 ml of concentrated hydrochloric acid was added to the reaction mixture and then the toluene layer was separated and washed with water. The toluene was distilled off under reduced pressure and the residual oily product was crystallized from methanol to obtain 77.1 g of ethyl p-isothiocyanatobenzoate. Yield: 74.5%. Melting Point: 52° C.
後処理
- temperaturethe mixture was refluxed
- temperatureby heating for 8 hours
- additionwas added to the reaction mixture
- customthe toluene layer was separated
- washwashed with water
- distillationThe toluene was distilled off under reduced pressure
- customthe residual oily product was crystallized from methanol
出典と根拠
- ORDレコード
- ord-c231143eab2a4a9290729ced9a8af7a9
- 出典データセット
- uspto-grants-1986_12
- 特許番号
- US04628024
反応ノート
読み込み中…