Hydrochloric Acid → Ethyl 4-isothiocyanatobenzoate

HRID 648897

반응식

HRID 648897 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 1140Toluene용매2회

실험 절차

In 500 ml of toluene was dissolved 82.5 g of ethyl p-aminobenzoate and after adding thereto 83.4 g of N,N-diethylthiocarbamoyl chloride, the mixture was refluxed for 8 hours. After ice cooling the reaction mixture, 100 ml of concentrated hydrochloric acid was added to the mixture and the toluene layer thus formed was collected and washed with water. After distilling off toluene under reduced pressure, the oily material thus formed was crystallized from methanol to provide 77.1 g of ethyl p-isothiocyanatobenzoate. The yield was 74.5% and the melting point was 52° C.

후처리

  1. additionafter adding
  2. customwas collected
  3. washwashed with water
  4. distillationAfter distilling off toluene under reduced pressure
  5. customthe oily material thus formed
  6. customwas crystallized from methanol

출처 및 근거

ORD 기록
ord-bfc673d5814d406188d69c33b4ccee85
출처 데이터셋
uspto-grants-1988_04
특허 번호
US04737452

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