Dimethyl Sulfoxide → HCID 19080752, 화합물

HRID 963166노트

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HRID 963166 반응식
N1C=CC=CC=1.CS(C)=O.Cl[S:12]([C:15]1[N:23]=[C:22]2[N:17]([C:18]([O:25][CH3:26])=[N:19][C:20]([CH3:24])=[CH:21]2)[N:16]=1)(=[O:14])=[O:13].[NH2:27][C:28]1[C:29]([C:36]([F:39])([F:38])[F:37])=[N:30][N:31]([CH2:34][CH3:35])[C:32]=1[CH3:33]>C(#N)C>[CH2:34]([N:31]1[C:32]([CH3:33])=[C:28]([NH:27][S:12]([C:15]2[N:23]=[C:22]3[N:17]([C:18]([O:25][CH3:26])=[N:19][C:20]([CH3:24])=[CH:21]3)[N:16]=2)(=[O:14])=[O:13])[C:29]([C:36]([F:38])([F:37])[F:39])=[N:30]1)[CH3:35]

참가 물질

6

반응물 4

HCID 679Dimethyl SulfoxideHCID 1049PyridineHCID 15003653HCID 15003653, 화합물HCID 19080768HCID 19080768, 화합물

생성물 1

HCID 19080752HCID 19080752, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

Pyridine (0.32 g (4.0 mmol)) and dimethyl sulfoxide (0.03 g (0.4 mmol)) were added to a solution of 1.0 g (4.0 mmol) of 2-chlorosulfonyl-5-methoxy-7-methyl[1,2,4]triazolo[1,5-c]pyrimidine and 0.77 g (4.0 mmol) of 4-amino-1-ethyl-5-methyl-3-(trifluoromethyl)pyrazole in 15 mL of acetonitrile at ambient temperature with stirring. After 18 hours, the volatiles were removed by evaporation under reduced pressure and the residue was partitioned between dichloromethane and water, stirring for 10 min before separation. The solids were recovered by filtration and washed with ether. They were then resuspended in water and the mixture stirred for 30 min. The solids were recovered by filtration, washed with ether, and dried under reduced pressure at 40° C. overnight. The resulting 1.3 g (78 percent of theory) of white powder melting at 208°-209° C. was the title compound (Compound 1).

후처리

  1. customthe volatiles were removed by evaporation under reduced pressure
  2. customthe residue was partitioned between dichloromethane and water
  3. stirringstirring for 10 min before separation
  4. filtrationThe solids were recovered by filtration
  5. washwashed with ether
  6. stirringthe mixture stirred for 30 min
  7. filtrationThe solids were recovered by filtration
  8. washwashed with ether
  9. customdried under reduced pressure at 40° C. overnight

출처 및 근거

ORD 기록
ord-a1dd11aa331a496db92e3f7c5a150765
출처 데이터셋
uspto-grants-1998_06
특허 번호
US05763359

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