Methylamine → (2-(Methylamino)pyridin-4-yl)methanol

HRID 1421063노트

반응식

HRID 1421063 반응식
Cl[C:2]1[CH:7]=[C:6]([CH2:8][OH:9])[CH:5]=[CH:4][N:3]=1.[CH3:10][NH2:11]>C(O)C>[OH:9][CH2:8][C:6]1[CH:5]=[CH:4][N:3]=[C:2]([NH:11][CH3:10])[CH:7]=1

참가 물질

4

반응물 2

HCID 6329MethylamineHCID 7062237(2-Chloropyridin-4-yl)methanol

생성물 1

HCID 22625034(2-(Methylamino)pyridin-4-yl)methanol수율 46%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
200 °C

실험 절차

A mixture of 2-chloro-4-hydroxymethylpyridine (1.0 g, 7 mmol), (prepared as described for the starting material in Example 58), and methylamine (30 ml of a 30% solution in ethanol) was heated in a Carius tube for 16 hours at 200° C. The mixture was allowed to cool and the mixture partitioned between saturated aqueous sodium hydrogen carbonate solution and ethyl acetate. The organic layer was separated, dried (MgSO4) and the volatiles removed by evaporation. The residue was purified by column chromatography eluting with ethyl acetate to give 4-hydroxymethyl-2-(methylamino)pyridine (440 mg, 46%) as a yellow oil.

후처리

  1. custom(prepared
  2. temperatureto cool
  3. customthe mixture partitioned between saturated aqueous sodium hydrogen carbonate solution and ethyl acetate
  4. customThe organic layer was separated
  5. dry with materialdried (MgSO4)
  6. customthe volatiles removed by evaporation
  7. customThe residue was purified by column chromatography
  8. washeluting with ethyl acetate

출처 및 근거

ORD 기록
ord-fcc78c5b65f0487798cbda2c0a8aad10
출처 데이터셋
uspto-grants-2000_06
특허 번호
US06071921

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