Hydrochloric Acid → Ethyl 4-isothiocyanatobenzoate

HRID 648897

反応式

HRID 648897 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2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-bfc673d5814d406188d69c33b4ccee85
出典データセット
uspto-grants-1988_04
特許番号
US04737452

関連ノート

読み込み中…