Triethylamine → HCID 178503424, 화합물

HRID 2359029노트

반응식

HRID 2359029 반응식
C[N:2](C)[CH:3]=[C:4]([C:13]1[CH:18]=[CH:17][N:16]=[C:15]([S:19][CH3:20])[N:14]=1)[C:5]([C:7]1[S:8][C:9]([Cl:12])=[CH:10][CH:11]=1)=O.O.NN.C([N:27](CC)CC)C>C(O)C.O>[Cl:12][C:9]1[S:8][C:7]([C:5]2[C:4]([C:13]3[CH:18]=[CH:17][N:16]=[C:15]([S:19][CH3:20])[N:14]=3)=[CH:3][NH:2][N:27]=2)=[CH:11][CH:10]=1

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 24654Hydrazine hydrate (1:1)HCID 67261197HCID 67261197, 화합물

생성물 1

HCID 178503424HCID 178503424, 화합물수율 81%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

To a mixture of 3-(dimethylamino)-1-(5-chloro-2-thienyl)-2-[2-(methylsulfanyl)pyrimidin-4-yl]prop-2-en-1-one (1 eq, 96 mmol) in 300 mL ethanol was added dropwise hydrazine hydrate (1.5 eq, 144 mmol) and then triethylamine (1.5 eq, 144 mmol). The mixture was heated under reflux for 2 h and then overnight at room temperature. The solvent was then slowly poured in 1 L of water. The resulting precipitate was filtered and dried to afford 24 g of 4-[3-(5-chloro-2-thienyl)-1H-pyrazol-4-yl]-2-(methylsulfanyl)pyrimidine (80% yield).

후처리

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 2 h
  3. customovernight
  4. customat room temperature
  5. filtrationThe resulting precipitate was filtered
  6. customdried

출처 및 근거

ORD 기록
ord-1a365012950c44fc84e93bc8fdf2f431
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08685974B2

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