Water → (6-Methylpyridin-3-yl)methanol

HRID 868339

反応式

HRID 868339 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][C:8]1[CH:18]=[CH:17][C:11]([C:12](OCC)=[O:13])=[CH:10][N:9]=1.O>C(OCC)C>[OH:13][CH2:12][C:11]1[CH:17]=[CH:18][C:8]([CH3:7])=[N:9][CH:10]=1

参加物

5

反応物 3

HCID 962WaterHCID 281994Ethyl 6-methylnicotinateHCID 21226445Aluminium lithium hydride2 回

生成物 1

HCID 11228788(6-Methylpyridin-3-yl)methanol収率 80.4%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

反応条件

温度
0 °C

実験手順

To a stirred suspension of 11.4 g of lithium aluminum hydride in 500 ml of dry diethyl ether, 32.7 g of ethyl 6-methylnicotinate in 250 ml of dry diethyl ether is added dropwise at room temperature, and the mixture is refluxed for 1.5 hours. The reaction mixture is cooled to 0° C., and the remaining lithium aluminum hydride is decomposed by the cautious addition of 60 ml of water. The ether layer is decanted, and the residual solid is extracted with three 150-ml portions of diethyl ether. The combined extracts are dried over potassium carbonate and concentrated to give 19.6 g of crude 5-hydroxymethyl-2-methylpyridine.

後処理

  1. additionis added dropwise at room temperature
  2. temperaturethe mixture is refluxed for 1.5 hours
  3. customThe ether layer is decanted
  4. extractionthe residual solid is extracted with three 150-ml portions of diethyl ether
  5. dry with materialThe combined extracts are dried over potassium carbonate
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-a207923c88b1460b814fb374ece9c4c5
出典データセット
uspto-grants-1988_10
特許番号
US04778796

関連ノート

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