Methylamine → (2-(Methylamino)pyridin-4-yl)methanol

HRID 1421063ノート

反応式

HRID 1421063 の反応式
Cl[C:2]1[CH:7]=[C:6]([CH2:8][OH:9])[CH:5]=[CH:4][N:3]=1.[CH3:10][NH2:11]>C(O)C>[OH:9][CH2:8][C:6]1[CH:5]=[CH:4][N:3]=[C:2]([NH:11][CH3:10])[CH:7]=1

参加物

4

反応物 2

HCID 6329MethylamineHCID 7062237(2-Chloropyridin-4-yl)methanol

生成物 1

HCID 22625034(2-(Methylamino)pyridin-4-yl)methanol収率 46%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
200 °C

実験手順

A mixture of 2-chloro-4-hydroxymethylpyridine (1.0 g, 7 mmol), (prepared as described for the starting material in Example 58), and methylamine (30 ml of a 30% solution in ethanol) was heated in a Carius tube for 16 hours at 200° C. The mixture was allowed to cool and the mixture partitioned between saturated aqueous sodium hydrogen carbonate solution and ethyl acetate. The organic layer was separated, dried (MgSO4) and the volatiles removed by evaporation. The residue was purified by column chromatography eluting with ethyl acetate to give 4-hydroxymethyl-2-(methylamino)pyridine (440 mg, 46%) as a yellow oil.

後処理

  1. custom(prepared
  2. temperatureto cool
  3. customthe mixture partitioned between saturated aqueous sodium hydrogen carbonate solution and ethyl acetate
  4. customThe organic layer was separated
  5. dry with materialdried (MgSO4)
  6. customthe volatiles removed by evaporation
  7. customThe residue was purified by column chromatography
  8. washeluting with ethyl acetate

出典と根拠

ORDレコード
ord-fcc78c5b65f0487798cbda2c0a8aad10
出典データセット
uspto-grants-2000_06
特許番号
US06071921

反応ノート

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