Hydrochloric Acid → 1-(2-Aminoethyl)-3-(2,6-dichlorophenyl)thiourea

HRID 243522

반응식

HRID 243522 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[N:9]=[C:10]=[S:11].C1COCC1.[CH2:17]([NH2:20])[CH2:18][NH2:19].Cl>O>[NH2:19][CH2:18][CH2:17][NH:20][C:10]([NH:9][C:3]1[C:2]([Cl:1])=[CH:7][CH:6]=[CH:5][C:4]=1[Cl:8])=[S:11]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 3301EthylenediamineHCID 8028Tetrahydrofuran2회HCID 1232391,3-Dichloro-2-isothiocyanatobenzene

생성물 1

HCID 30367871-(2-Aminoethyl)-3-(2,6-dichlorophenyl)thiourea

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A solution of 2,6-dichlorophenyl isothiocyanate (500 mg) and THF (5 ml) was added dropwise under argon within 20 minutes to a solution of ethylenediamine (3.68 g) and abs. THF (4 ml). After stirring for a further 30 min, the mixture was added to water, acidified with 10% HCl and extracted three times with ethyl acetate. The aqueous phase was made basic using saturated potassium carbonate solution, and extracted three times with ethyl acetate. The combined organic phases were dried over magnesium sulfate, the solvent was removed under reduced pressure and the residue was co-evaporated twice with toluene. After drying in high vacuum, the desired product was obtained as a white solid (532 mg).

후처리

  1. extractionextracted three times with ethyl acetate
  2. extractionextracted three times with ethyl acetate
  3. dry with materialThe combined organic phases were dried over magnesium sulfate
  4. customthe solvent was removed under reduced pressure
  5. customAfter drying in high vacuum

출처 및 근거

ORD 기록
ord-0c9352ce51844b3ab9f9a5a1d8a82163
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08653259B2

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