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Triethylamine → 2-(4-Chloro-3,5-dimethoxyphenyl)-4-hydroxymethylpyridine

HRID 2300310
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HRID 2300310 반응식
[Cl:1][C:2]1[C:7]([O:8][CH3:9])=[CH:6][C:5]([C:10]2[CH:11]=[C:12]([CH:16]=[CH:17][N:18]=2)[C:13](O)=[O:14])=[CH:4][C:3]=1[O:19][CH3:20].C(N(CC)CC)C.ClC(OCC)=O>C1COCC1>[Cl:1][C:2]1[C:3]([O:19][CH3:20])=[CH:4][C:5]([C:10]2[CH:11]=[C:12]([CH2:13][OH:14])[CH:16]=[CH:17][N:18]=2)=[CH:6][C:7]=1[O:8][CH3:9]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 225580392-(4-Chloro-3,5-dimethoxyphenyl)isonicotinic acid

생성물 1

HCID 225579712-(4-Chloro-3,5-dimethoxyphenyl)-4-hydroxymethylpyridine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To an ice-cooled solution of 2-(4-chloro-3,5-dimethoxyphenyl)isonicotinic acid (7.20 g) and triethylamine (5.6 mL) in THF (70 mL) was added ethyl chloroformate (2.8 mL). The mixture was stirred at room temperature for 1 hour and filtered. To the filtrate was then added a solution of sodium borohydride (1.25 g) in water (4 mL). The mixture was stirred at room temperature for another hour and evaporated. Water was added to the residue and extracted with chloroform. The organic layer was washed with brine, dried over anhydrous sodium sulfate and evaporated. The residue was subjected to silica gel column chromatography using chloroform-methanol (20:1) and then chloroform-methanol (15:1) to give the title compound.

후처리

  1. filtrationfiltered
  2. additionTo the filtrate was then added a solution of sodium borohydride (1.25 g) in water (4 mL)
  3. stirringThe mixture was stirred at room temperature for another hour
  4. customevaporated
  5. additionWater was added to the residue
  6. extractionextracted with chloroform
  7. washThe organic layer was washed with brine
  8. dry with materialdried over anhydrous sodium sulfate
  9. customevaporated

출처 및 근거

ORD 기록
ord-2d1446de7302479dbabfad3360485e1d
출처 데이터셋
uspto-grants-2002_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06498169B1

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