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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Potassium Carbonate → 5,7-dihydro-5,5,7,7-tetramethyl-2-[[(3-methyl-4-nitro-2-pyridyl)methyl]thio]indeno[5,6-d]imidazol-6(1H)-one

HRID 35450
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HRID 35450 반응식
Cl[CH2:2][C:3]1[C:8]([CH3:9])=[C:7]([N+:10]([O-:12])=[O:11])[CH:6]=[CH:5][N:4]=1.[SH:13][C:14]1[NH:18][C:17]2[CH:19]=[C:20]3[C:24](=[CH:25][C:16]=2[N:15]=1)[C:23]([CH3:27])([CH3:26])[C:22](=[O:28])[C:21]3([CH3:30])[CH3:29].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[CH3:29][C:21]1([CH3:30])[C:20]2[C:24](=[CH:25][C:16]3[NH:15][C:14]([S:13][CH2:2][C:3]4[C:8]([CH3:9])=[C:7]([N+:10]([O-:12])=[O:11])[CH:6]=[CH:5][N:4]=4)=[N:18][C:17]=3[CH:19]=2)[C:23]([CH3:27])([CH3:26])[C:22]1=[O:28]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 160959042-(Chloromethyl)-3-methyl-4-nitropyridineHCID 178429018HCID 178429018, 화합물

생성물 1

HCID 221514395,7-dihydro-5,5,7,7-tetramethyl-2-[[(3-methyl-4-nitro-2-pyridyl)methyl]thio]indeno[5,6-d]imidazol-6(1H)-one

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A solution of 11,5 g (0.062 mol) of 2-chloromethyl-3 -methyl-4-nitropyridine and 16 g (0.06 mol) of 5,7-dihydro-2-mercapto-5,5,7,7-tetramethylindeno[5,6-d]-imidazol-6(1H)-one in 200 ml of abs. acetone is treated with 13 g of finely ground potassium carbonate and the mixture is stirred at room temperature under argon for 18 hours, 100 ml of acetone are distilled off in vacuo, whereupon the residue is poured on to ice. The product which crystallizes out is filtered off and dissolved in methylene chloride; the solution obtained is washed with water, dried and concentrated. By recrystallization from ethyl acetate/ether there is obtained 5,7-dihydro-5,5,7,7-tetramethyl-2 -[[(3-methyl-4-nitro-2 -pyridyl)methyl]thio]indeno[5,6-d]imidazol-6(1H)-one of melting point 181°-183° (decomposition).

후처리

  1. distillation100 ml of acetone are distilled off in vacuo, whereupon the residue
  2. additionis poured on to ice
  3. customThe product which crystallizes out
  4. filtrationis filtered off
  5. dissolutiondissolved in methylene chloride
  6. customthe solution obtained
  7. washis washed with water
  8. customdried
  9. concentrationconcentrated
  10. customBy recrystallization from ethyl acetate/ether there

출처 및 근거

ORD 기록
ord-290a559b7d5e464db1ce918e68b2764b
출처 데이터셋
uspto-grants-1988_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04766133

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