Triethylamine → HCID 178503424、化合物

HRID 2359029ノート

反応式

HRID 2359029 の反応式
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

参加物

6

反応物 3

HCID 8471TriethylamineHCID 24654Hydrazine hydrate (1:1)HCID 67261197HCID 67261197、化合物

生成物 1

HCID 178503424HCID 178503424、化合物収率 81%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-1a365012950c44fc84e93bc8fdf2f431
出典データセット
uspto-grants-2014_04
特許番号
US08685974B2

反応ノート

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