Sodium Chloride → 6-Chloro-5-methyl-2-pyridinemethanol

HRID 376299ノート

反応式

HRID 376299 の反応式
[BH4-].[Na+].C([O:5][C:6]([C:8]1[CH:13]=[CH:12][C:11]([CH3:14])=[C:10]([Cl:15])[N:9]=1)=O)C.[Cl-].[Na+]>C(O)C>[Cl:15][C:10]1[N:9]=[C:8]([CH2:6][OH:5])[CH:13]=[CH:12][C:11]=1[CH3:14]

参加物

5

反応物 3

HCID 5234Sodium ChlorideHCID 4311764Sodium borohydrideHCID 9837074Ethyl 6-chloro-5-methylpicolinate

生成物 1

HCID 104871386-Chloro-5-methyl-2-pyridinemethanol収率 73%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

0.40 g of sodium borohydride (10.5 mmol) is added in portions to a solution of 1.20 g of 6-chloro-5-methylpyridine-2-carboxylic acid ethyl ester (6.00 mmol) and 10 ml of ethanol maintained at room temperature. The mixture is stirred for 4 hours and then the mixture is poured into an aqueous solution of sodium chloride and the mixture is extracted with ethyl acetate. The organic phase is dried over sodium sulfate, filtered and concentrated under vacuum. The title product is isolated by chromatography on a silica column (eluent: chloroform). 0.69 g of a colorless oil is recovered.

後処理

  1. extractionthe mixture is extracted with ethyl acetate
  2. dry with materialThe organic phase is dried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-985e6d9e57ba4ff29986cc6b195b8960
出典データセット
uspto-grants-2000_02
特許番号
US06020345

反応ノート

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