Methanol → HCID 54724774, 화합물

HRID 2216400노트

반응식

HRID 2216400 반응식
[Na].CO.[C:4]([O:8][CH3:9])(=[O:7])[CH2:5][SH:6].Cl[C:11]1[C:16]([C:17](OCC)=[O:18])=[CH:15][CH:14]=[C:13]([CH:22]([CH3:24])[CH3:23])[N:12]=1>CN(C)C=O.O>[CH3:9][O:8][C:4]([C:5]1[S:6][C:11]2=[N:12][C:13]([CH:22]([CH3:23])[CH3:24])=[CH:14][CH:15]=[C:16]2[C:17]=1[OH:18])=[O:7]

참가 물질

7

반응물 4

HCID 887MethanolHCID 16907Methyl ThioglycolateHCID 5360545SodiumHCID 21942344Ethyl 2-chloro-6-(propan-2-yl)pyridine-3-carboxylate

생성물 1

HCID 54724774HCID 54724774, 화합물수율 45.1%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

Under ice-cooling, metal sodium (6.9 g) was added to methanol (70 ml)-and methyl thioglycolate (32 g) was added with stirring. Ethyl 2-chloro-6-isopropylpyridine-3-carboxylate (42 g) synthesized according to U.S. Pat. No. 5,001,137 (Mar. 19, 1991) was dissolved in dimethylformamide (170 ml) and the mixture was stirred at room temperature for 2 hr. The reaction mixture was treated with water, and the organic layer was extracted with ethyl acetate, washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The obtained crystals were recrystallized from water-containing methanol to give the title compound (20.9 g). melting point: 80-81° C.

후처리

  1. temperatureUnder ice-cooling
  2. additionwas added
  3. stirringthe mixture was stirred at room temperature for 2 hr
  4. extractionthe organic layer was extracted with ethyl acetate
  5. washwashed with saturated brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customThe solvent was evaporated under reduced pressure
  8. customThe obtained crystals were recrystallized from water-
  9. additioncontaining methanol

출처 및 근거

ORD 기록
ord-09dd42b327c647939bde6cc37a318ae4
출처 데이터셋
uspto-grants-2006_09
특허 번호
US07112594B2

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