Ethanol → O-Ethyl (3-Chlorophenyl)-thiocarbamate

HRID 223395

反応式

HRID 223395 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([N:8]=[C:9]=[S:10])[CH:5]=[CH:6][CH:7]=1.N1C2C(=CC=CC=2)C=CC=1.[CH2:21]([OH:23])[CH3:22]>>[Cl:1][C:2]1[CH:3]=[C:4]([NH:8][C:9](=[S:10])[O:23][CH2:21][CH3:22])[CH:5]=[CH:6][CH:7]=1

参加物

4

反応物 3

HCID 702EthanolHCID 7047QuinolineHCID 754493-Chlorophenyl isothiocyanate

生成物 1

HCID 54084842O-Ethyl (3-Chlorophenyl)-thiocarbamate

実験手順

A mixture of 45.5 gm (0.268 mol) of 3-chlorophenylisothiocyanate, 200 ml of anhydrous ethanol and 1 ml of quinoline was refluxed for 48 hours. Then, the reaction mixture was evaporated in an aspirator vacuum, the residue was taken up in ether, and the resulting solution was washed first with 5% hydrochloric acid and then thoroughly with water, dried, and evaporated again. After recrystallization from methanol/water, 49.5 gm (86% of theory) of colorless crystals with a melting point of 78°-79° C. were obtained.

後処理

  1. temperaturewas refluxed for 48 hours
  2. customThen, the reaction mixture was evaporated in an aspirator vacuum
  3. washthe resulting solution was washed first with 5% hydrochloric acid
  4. dry with materialthoroughly with water, dried
  5. customevaporated again
  6. customAfter recrystallization from methanol/water, 49.5 gm (86% of theory) of colorless crystals with a melting point of 78°-79° C.
  7. customwere obtained

出典と根拠

ORDレコード
ord-0314404d9a3246f4a990bc889874e10e
出典データセット
uspto-grants-1982_10
特許番号
US04353919

関連ノート

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