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

HRID 243522

反応式

HRID 243522 の反応式
[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]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 3301EthylenediamineHCID 8028Tetrahydrofuran2 回HCID 1232391,3-Dichloro-2-isothiocyanatobenzene

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-0c9352ce51844b3ab9f9a5a1d8a82163
出典データセット
uspto-grants-2014_02
特許番号
US08653259B2

関連ノート

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