Water → HCID 17862916, 화합물

HRID 1172136노트

반응식

HRID 1172136 반응식
[Cl:1][C:2]1[N:11]=[CH:10][CH:9]=[C:8]([CH3:12])[C:3]=1[C:4](OC)=[O:5].[H-].[Al+3].[Li+].[H-].[H-].[H-].O>C1COCC1>[Cl:1][C:2]1[C:3]([CH2:4][OH:5])=[C:8]([CH3:12])[CH:9]=[CH:10][N:11]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 17862852Methyl 2-chloro-4-methylpyridine-3-carboxylateHCID 21226445Aluminium lithium hydride

생성물 1

HCID 17862916HCID 17862916, 화합물수율 38.2%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
-20 °C

실험 절차

A solution of 1.9 g (10.0 mmoles) of methyl 2-chloro-4-methylnicotinate dissolved in 5.0 ml of THF was gradually added, at −65 to −60° C., to a suspension of 0.4 g (10.0 mmoles) of lithium aluminum hydride in 30 ml of tetrahydrofuran. The mixture was stirred for 30 minutes and at −20° C. for 1 hour to give rise to a reaction. The reaction mixture was poured into water, followed by extraction with ethyl acetate. The resulting organic layer was washed with water and an aqueous sodium chloride solution in this order and then dried over anhydrous magnesium sulfate. The resulting solution was subjected to vacuum distillation to remove the solvent contained therein. The residue was purified by silica gel column chromatography to obtain 0.6 g (yield: 38.2%) of (2-chloro-4-methylpyridin-3-yl)methanol.

후처리

  1. customto give rise
  2. customto a reaction
  3. extractionfollowed by extraction with ethyl acetate
  4. washThe resulting organic layer was washed with water
  5. dry with materialan aqueous sodium chloride solution in this order and then dried over anhydrous magnesium sulfate
  6. distillationThe resulting solution was subjected to vacuum distillation
  7. customto remove the solvent
  8. customThe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-8e4f69a4015244c984571d40bbe54b4c
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07833939B2

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