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

HRID 376299노트

반응식

HRID 376299 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 104871386-Chloro-5-methyl-2-pyridinemethanol수율 73%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-985e6d9e57ba4ff29986cc6b195b8960
출처 데이터셋
uspto-grants-2000_02
특허 번호
US06020345

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