Hydrochloric Acid → Ethyl 4-isothiocyanatobenzoate

HRID 1248958노트

반응식

HRID 1248958 반응식
[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]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 2337BenzocaineHCID 66607Diethylthiocarbamoyl chloride

생성물 1

HCID 71003Ethyl 4-isothiocyanatobenzoate수율 74.5%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.

후처리

  1. temperaturethe mixture was refluxed
  2. temperatureby heating for 8 hours
  3. additionwas added to the reaction mixture
  4. customthe toluene layer was separated
  5. washwashed with water
  6. distillationThe toluene was distilled off under reduced pressure
  7. customthe residual oily product was crystallized from methanol

출처 및 근거

ORD 기록
ord-c231143eab2a4a9290729ced9a8af7a9
출처 데이터셋
uspto-grants-1986_12
특허 번호
US04628024

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