Hydrochloric Acid → Ethyl 4-isothiocyanatobenzoate

HRID 1248958

反応式

HRID 1248958 の反応式
[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

反応物 3

HCID 313Hydrochloric AcidHCID 2337BenzocaineHCID 66607Diethylthiocarbamoyl chloride

生成物 1

HCID 71003Ethyl 4-isothiocyanatobenzoate収率 74.5%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

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

  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

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

関連ノート

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