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Sodium methanethiolate → 8-(2,6-Dimethylbenzylamino)-3-methyl-2-methylsulfanylmethyl-imidazo[1,2-a]pyridine

HRID 1369566
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HRID 1369566 반응식
Cl[CH2:2][C:3]1[N:4]=[C:5]2[C:10]([NH:11][CH2:12][C:13]3[C:18]([CH3:19])=[CH:17][CH:16]=[CH:15][C:14]=3[CH3:20])=[CH:9][CH:8]=[CH:7][N:6]2[C:21]=1[CH3:22].[CH3:23][S-:24].[Na+]>C(#N)C>[CH3:20][C:14]1[CH:15]=[CH:16][CH:17]=[C:18]([CH3:19])[C:13]=1[CH2:12][NH:11][C:10]1[C:5]2[N:6]([C:21]([CH3:22])=[C:3]([CH2:2][S:24][CH3:23])[N:4]=2)[CH:7]=[CH:8][CH:9]=1
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참가 물질

4

반응물 2

HCID 4378561Sodium methanethiolateHCID 226726282-Chloromethyl-8-(2,6-dimethylbenzylamino)-3-methylimidazo[1,2-a]pyridine

생성물 1

HCID 226726258-(2,6-Dimethylbenzylamino)-3-methyl-2-methylsulfanylmethyl-imidazo[1,2-a]pyridine수율 24%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

2-chloromethyl-8-(2,6-dimethylbenzylamino)-3-methylimidazo[1,2-a]pyridine (0.2 g, 0.64 mmol) and sodium methanethiolate (0.1 g, 1.3 mmol) were added to acetonitrile(10 ml) and stirred for 4 h. at room temperature. The solvent was evaporated under reduced pressure and to the residue were added methylene chloride and water. The organic layer was separated, dried (Na2SO4) and evaporated under reduced pressure. Purification of the residue by column chromatography on silica gel using diethyl ether:petroleum ether (1:2) as eluent and crystallization from diethyl ether:petroleum ether (1:2) gave 0.05 g (24%) of the desired product.

후처리

  1. customThe solvent was evaporated under reduced pressure and to the residue
  2. additionwere added methylene chloride and water
  3. customThe organic layer was separated
  4. dry with materialdried (Na2SO4)
  5. customevaporated under reduced pressure
  6. customPurification of the residue by column chromatography on silica gel
  7. customcrystallization from diethyl ether:petroleum ether (1:2)

출처 및 근거

ORD 기록
ord-473027edc42c425b9c970490909efdc5
출처 데이터셋
uspto-grants-2003_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06579884B1

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