Thionyl Chloride → N-(2-chloroethyl)-2-pyridinecarboxamide hydrochloride

HRID 437651ノート

反応式

HRID 437651 の反応式
O[CH2:2][CH2:3][NH:4][C:5]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][N:8]=1)=[O:6].S(Cl)([Cl:15])=O>>[ClH:15].[Cl:15][CH2:2][CH2:3][NH:4][C:5]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][N:8]=1)=[O:6]

参加物

3

反応物 2

HCID 24386Thionyl ChlorideHCID 2045999N-(2-Hydroxyethyl)picolinamide

生成物 1

HCID 21428902N-(2-chloroethyl)-2-pyridinecarboxamide hydrochloride

実験手順

To 49 parts of N-(2-hydroxyethyl)-2-pyridinecarboxamide are added dropwise 80 parts of sulfinyl chloride while stirring vigourously. Upon completion, stirring is continued first for 3 hours at reflux and further for 2 hours at room temperature. The excess of sulfinyl chloride is evaporated and the residue is poured onto hot methanol. After cooling, the precipitated product is filtered off (the filtrate is set aside) and washed thoroughly with 2,2'-oxybispropane, yielding a first fraction of 14 parts of N-(2-chloroethyl)-2-pyridinecarboxamide hydrochloride.

後処理

  1. stirringUpon completion, stirring
  2. customThe excess of sulfinyl chloride is evaporated
  3. additionthe residue is poured onto hot methanol
  4. temperatureAfter cooling
  5. filtrationthe precipitated product is filtered off (the filtrate
  6. washwashed thoroughly with 2,2'-oxybispropane

出典と根拠

ORDレコード
ord-d29d4b933f24494d889baec150191e36
出典データセット
uspto-grants-1977_06
特許番号
US04031226

反応ノート

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