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Triethylamine → HCID 178461109, 화합물

HRID 1182895
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HRID 1182895 반응식
C(N(CC)CC)C.[C:8]([C@@H:12]1[CH2:17][CH2:16][C@H:15]([NH2:18])[CH2:14][CH2:13]1)([CH3:11])([CH3:10])[CH3:9].[F:19][CH:20]([C:22]1[C:27]([Cl:28])=[C:26](Cl)[N:25]2[N:30]=[CH:31][N:32]=[C:24]2[N:23]=1)[CH3:21]>[I-].C([N+](CCCC)(CCCC)CCCC)CCC.C1(C)C=CC=CC=1>[C:8]([C@@H:12]1[CH2:13][CH2:14][C@H:15]([NH:18][C:26]2[N:25]3[N:30]=[CH:31][N:32]=[C:24]3[N:23]=[C:22]([CH:20]([F:19])[CH3:21])[C:27]=2[Cl:28])[CH2:16][CH2:17]1)([CH3:11])([CH3:9])[CH3:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 860365495-(1-Fluoroethyl)-6,7-dichloro-[1,2,4]triazolo[1,5-a]pyrimidineHCID 178445676HCID 178445676, 화합물

생성물 1

HCID 178461109HCID 178461109, 화합물

시약·촉매·용매 2

HCID 67553Tetrabutylammonium Iodide촉매HCID 1140Toluene
용매

실험 절차

0.220 g (2.2 mmol) Triethylamine, a spatula tip of tetrabutylammonium iodide and 0.340 g (2.2 mmol) of cis-4-tert-butylcyclohexylamine were added successively to a solution of 0.470 g (2.0 mmol) of 5-(1-fluoroethyl)-6,7-dichloro-[1,2,4]triazolo[1,5-a]pyrimidine in 15 ml of toluene under stirring. The reaction mixture was heated at reflux for 5 hours and then stirred for another 12 hours at room temperature. The solvent was evaporated under reduced pressure and dichloromethane was added to the resulting residue. The resulting reaction mixture was washed with 2N hydrochloric acid and water. The organic phase was separated, dried and the solvent was evaporated under reduced pressure. Treatment of the resulting residue with hexane yielded 0.540 g (1.5 mmol, 76% of theory) of the title compound having a melting point of 138-139° C.

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux for 5 hours
  3. stirringstirred for another 12 hours at room temperature
  4. customThe solvent was evaporated under reduced pressure and dichloromethane
  5. additionwas added to the resulting residue
  6. customThe resulting reaction mixture
  7. washwas washed with 2N hydrochloric acid and water
  8. customThe organic phase was separated
  9. customdried
  10. customthe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-b3856b4e115446bdb110b713d9e0fb18
출처 데이터셋
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08664235B2

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