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

HRID 437651노트

반응식

HRID 437651 반응식
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]

참가 물질

3

반응물 2

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

생성물 1

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

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d29d4b933f24494d889baec150191e36
출처 데이터셋
uspto-grants-1977_06
특허 번호
US04031226

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