Potassium Carbonate → HCID 178504129、化合物

HRID 1192947ノート

反応式

HRID 1192947 の反応式
Br[CH2:2][C:3]1[C:4]([C:14]([F:17])([F:16])[F:15])=[N:5][N:6](C)[C:7]=1[O:8][CH:9]1[CH2:12][O:11][CH2:10]1.NC(N)=S.[CH3:22][S:23]([C:26]1[CH2:30][C:29]([CH3:32])([CH3:31])[O:28][N:27]=1)(=O)=O.C(=O)([O-])[O-].[K+].[K+]>C(O)C>[CH3:31][C:29]1([CH3:32])[O:28][N:27]=[C:26]([SH:23]([CH2:2][C:3]2[C:4]([C:14]([F:17])([F:16])[F:15])=[N:5][NH:6][C:7]=2[O:8][CH:9]2[CH2:12][O:11][CH2:10]2)[CH3:22])[CH2:30]1

参加物

6

反応物 4

HCID 11430Potassium CarbonateHCID 2723790ThioureaHCID 121376563-Methylsulfonyl-5,5-dimethyl-2-isoxazolineHCID 597396184-bromomethyl-1-methyl-5-(oxetan-3-yloxy)-3-trifluoromethyl-1H-pyrazole

生成物 1

HCID 178504129HCID 178504129、化合物収率 34%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

4-Bromomethyl-1-methyl-5-(oxetan-3-yloxy)-3-trifluoromethyl-1H-pyrazole (10.1 g, 32.2 mmol) and thiourea (2.7 g, 35.5 mmol) were stirred in ethanol (100 ml) at room temperature until the solids were dissolved. 3-Methanesulfonyl-5,5-dimethyl-4,5-dihydroisoxazole (6.28 g, 35.5 mmol) and potassium carbonate (4.91 g, 35.5 mmol) were added and the mixture was heated under reflux for 2 hours. The mixture was concentrated and purified by chromatography (eluent: ethyl acetate/hexane) to give the product as a white solid (4 g, 34% yield over two steps).

後処理

  1. dissolutionwere dissolved
  2. temperaturethe mixture was heated
  3. temperatureunder reflux for 2 hours
  4. concentrationThe mixture was concentrated
  5. custompurified by chromatography (eluent: ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-d1d5a38449df445d8037b7812dd88b8f
出典データセット
uspto-grants-2014_03
特許番号
US08680290B2

反応ノート

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