Sodium Methoxide → HCID 21490891、化合物

HRID 1973894ノート

反応式

HRID 1973894 の反応式
[OH:1][CH2:2][C:3]1[CH:8]=[C:7]([Cl:9])[C:6]([CH2:10][CH2:11][CH2:12][CH3:13])=[C:5]([Cl:14])[N:4]=1.[CH3:15][O-:16].[Na+]>CO>[OH:1][CH2:2][C:3]1[CH:8]=[C:7]([Cl:9])[C:6]([CH2:10][CH2:11][CH2:12][CH3:13])=[C:5]([O:16][CH3:15])[N:4]=1.[OH:1][CH2:2][C:3]1[CH:8]=[C:7]([O:16][CH3:15])[C:6]([CH2:10][CH2:11][CH2:12][CH3:13])=[C:5]([Cl:14])[N:4]=1

参加物

5

反応物 2

HCID 10942334Sodium MethoxideHCID 21490887HCID 21490887、化合物

生成物 2

HCID 21490891HCID 21490891、化合物HCID 21490913HCID 21490913、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

A solution of 103 g (0.44 mol) of 2-hydroxymethyl-4,6dichloro-5-n-butyl-pyridine in 100 ml of methanol is added dropwise over the course of 15 minutes, whilst stirring, to a solution of 59.4 g (1.1 mol) of sodium methylate in 500 ml of methanol. After completion of the addition, the reaction mixture is heated for 56 hours under reflux. It is then evaporated to dryness and the residue is suspended in ether. After filtration, the ether filtrate is dried by means of sodium sulphate, filtered and evaporated. Fractional distillation of the residue in a high vacuum yields 2-hydroxymethyl-4-chloro-5-n-butyl-6-methoxy-pyridine of the formula ##STR10## of boiling point 95°-98° (0.06 mm Hg) and 2-hydroxymethyl-4-methoxy-5-n-butyl-6-chloro-pyridine of the formula ##STR11## of boiling point 130°-134° (0.03 mm Hg).

後処理

  1. additionAfter completion of the addition
  2. temperaturethe reaction mixture is heated for 56 hours
  3. temperatureunder reflux
  4. customIt is then evaporated to dryness
  5. filtrationAfter filtration
  6. dry with materialthe ether filtrate is dried by means of sodium sulphate
  7. filtrationfiltered
  8. customevaporated
  9. distillationFractional distillation of the residue in a high vacuum

出典と根拠

ORDレコード
ord-bf8d8e5d0da84eb097b47a79715baaec
出典データセット
uspto-grants-1976_12
特許番号
US03998955

反応ノート

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