Water → N-(2-Aminoethyl)-N'(3,5-dimethoxyphenyl)thiourea

HRID 1193523

반응식

HRID 1193523 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([N:11]=[C:12]=[S:13])[CH:6]=[C:7]([O:9][CH3:10])[CH:8]=1.[CH2:14]([NH2:17])[CH2:15][NH2:16].O>CCOCC>[NH2:16][CH2:15][CH2:14][NH:17][C:12]([NH:11][C:5]1[CH:6]=[C:7]([O:9][CH3:10])[CH:8]=[C:3]([O:2][CH3:1])[CH:4]=1)=[S:13]

참가 물질

5

반응물 3

HCID 962WaterHCID 3301EthylenediamineHCID 1454223,5-Dimethoxyphenyl isothiocyanate

생성물 1

HCID 13604911N-(2-Aminoethyl)-N'(3,5-dimethoxyphenyl)thiourea

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

온도
50 °C

실험 절차

A slurry of 9.75 g (0.05 mole) of 3,5-dimethoxyphenyl isothiocyanate in 27 ml of ether was added dropwise to a stirred solution of 3.0 g (0.05 mole) of ethylenediamine at room temperature. A five-degree rise in temperature was noted at the start of the one hour addition period. A solid appeared during the addition, and stirring was continued for 2.5 hours. The batch was allowed to stand overnight, and 100 ml of H2O was added. The solid was removed by filtration and the filtrate acidified with 4.5 ml of concentrated HCl and evaporated to dryness on the steam bath. The residue was sonicated with 100 ml of water and warmed to 50° C. for 10 minutes. This was filtered and basified to pH 10 with 10% NaOH. This gave 2.6 g of 14, m.p. 125°-126° C. Analysis satisfactory for C11H17N3O2S.

후처리

  1. additionA five-degree rise in temperature was noted at the start of the one hour addition period
  2. additionA solid appeared during the addition
  3. waitto stand overnight
  4. customThe solid was removed by filtration
  5. customevaporated to dryness on the steam bath
  6. customThe residue was sonicated with 100 ml of water
  7. filtrationThis was filtered

출처 및 근거

ORD 기록
ord-55c9c6c8b341407bb24a3bb2999b6d79
출처 데이터셋
uspto-grants-1989_03
특허 번호
US04810725

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