Methanol → 4-Dimethylaminomethyl-2-hydroxymethylpyridine

HRID 1904075

반응식

HRID 1904075 반응식
S(OOS([O-])(=O)=O)([O-])(=O)=O.[NH4+].[NH4+].[CH3:13][N:14]([CH2:16][C:17]1[CH:22]=[CH:21][N:20]=[CH:19][CH:18]=1)[CH3:15].[CH3:23][OH:24].S(=O)(=O)(O)O>O>[CH3:13][N:14]([CH2:16][C:17]1[CH:22]=[CH:21][N:20]=[C:19]([CH2:23][OH:24])[CH:18]=1)[CH3:15]

참가 물질

6

반응물 4

HCID 887MethanolHCID 1118Sulfuric AcidHCID 62648Ammonium PersulfateHCID 2649464-pyridinemethanamine, N,N-dimethyl-

생성물 1

HCID 132926014-Dimethylaminomethyl-2-hydroxymethylpyridine

시약·촉매·용매 1

HCID 962Water용매3회

실험 절차

Ammonium persulphate (102.7 g) in water (200 ml) was added over 40 minutes to a refluxing solution of 4-dimethylaminomethylpyridine (40.86 g), methanol (450 ml), water (210 ml) and concentrated sulphuric acid (30 ml). The resulting solution was refluxed for 2 hours, water (300 ml) was added and the methanol was distilled off. The cooled solution was basified and extracted with chloroform to give 4-dimethylaminomethyl-2-hydroxymethylpyridine (19.65 g) b.p. 92°-120°/0.06 mm Hg.

후처리

  1. temperatureThe resulting solution was refluxed for 2 hours
  2. distillationthe methanol was distilled off
  3. extractionextracted with chloroform

출처 및 근거

ORD 기록
ord-c7eefca3e0a14bd684887e664777da8b
출처 데이터셋
uspto-grants-1984_03
특허 번호
US04439609

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