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Methanol → (3-Methoxypyridin-2-yl)methanol

HRID 262453
ノート
印刷プレビュー

反応式

HRID 262453 の反応式
[BH4-].[Na+].[CH3:3][O:4][C:5]1[C:6]([C:11](OC)=[O:12])=[N:7][CH:8]=[CH:9][CH:10]=1.CO>C(O)C>[OH:12][CH2:11][C:6]1[C:5]([O:4][CH3:3])=[CH:10][CH:9]=[CH:8][N:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 887MethanolHCID 4311764Sodium borohydride2 回HCID 20474189Methyl 3-methoxypyridine-2-carboxylate

生成物 1

HCID 5324774(3-Methoxypyridin-2-yl)methanol収率 57.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Sodium borohydride (6.3 g) was added slowly over 75 minutes to a solution of 3-methoxy-2-methoxycarbonylpyridine (9.2 g) in ethanol. Methanol (100 ml) was then added and after the initial vigorous reaction had subsided, further sodium borohydride (8.3 g) was added over a further 3 hours, and the mixture was left to stand overnight. The solvent was evaporated, the residue dissolved in water and extracted with chloroform and the chloroform solution dried. Evaporation, and crystallisation from ether gave 2-hydroxymethyl-3-methoxypyridine (4.4 g) m.p. 72.5°-73.5°.

後処理

  1. customafter the initial vigorous reaction
  2. waitthe mixture was left
  3. customThe solvent was evaporated
  4. dissolutionthe residue dissolved in water
  5. extractionextracted with chloroform
  6. dry with materialthe chloroform solution dried
  7. customEvaporation, and crystallisation from ether

出典と根拠

ORDレコード
ord-72680b78a511439cb77fa07e56c442ac
出典データセット
uspto-grants-1979_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04154838

反応ノート

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