Water → HCID 18936813, 화합물

HRID 357008

반응식

HRID 357008 반응식
[H-].[Na+].Cl.Cl[C:5]1[N:10]2[CH:11]=[CH:12][N:13]=[C:9]2[CH:8]=[CH:7][CH:6]=1.[OH:14][CH2:15][CH2:16][CH2:17][CH2:18][O:19][Si](C(C)(C)C)(C)C.O>CS(C)=O>[OH:14][CH2:15][CH2:16][CH2:17][CH2:18][O:19][C:5]1[N:10]2[CH:11]=[CH:12][N:13]=[C:9]2[CH:8]=[CH:7][CH:6]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 24758Sodium hydrideHCID 1864034-(Dimethyl-tert-butylsilyl)oxybutan-1-olHCID 219941745-Chloroimidazo[1,2-a]pyridine hydrochloride

생성물 1

HCID 18936813HCID 18936813, 화합물

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

In a nitrogen stream, 8.0 g (200 mmol) of 60% oily sodium hydride was added to a solution of 18.90 g (100 mmol) of 5-chloroimidazo[1,2-a]pyridine hydrochloride in 200 ml of dimethyl sulfoxide at 0° C., followed by stirring for 15 minutes. To this mixture, 20.44 g (100 mmol) of 4-hydroxy-1-t-butyldimethylsiloxybutane was added, followed by stirring room temperature for 5 hours. The reaction mixture was poured into water and extracted with ethyl acetate. The organic layer was washed with water and dried, after which the solvent was distilled off. The residue was purified by column chromatography (eluent: ethyl acetate) to yield 3.73 g (11.6%, orange oily substance) of the desired product.

후처리

  1. stirringby stirring room temperature for 5 hours
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with water
  4. customdried
  5. distillationafter which the solvent was distilled off
  6. customThe residue was purified by column chromatography (eluent: ethyl acetate)

출처 및 근거

ORD 기록
ord-3dc2156c8ccc40a8a198198e69ef81ad
출처 데이터셋
uspto-grants-1998_11
특허 번호
US05840732

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