Acetic Acid → HCID 178491357、化合物

HRID 1971446

反応式

HRID 1971446 の反応式
[CH3:1][O:2][C:3]1[CH:16]=[CH:15][CH:14]=[C:13]([O:17][CH3:18])[C:4]=1[CH2:5][NH:6][C:7](=[NH:12])[NH:8][C:9]([NH2:11])=[S:10].[F:19][C:20]([F:32])([F:31])[C:21]1[CH:30]=[CH:29][C:24]([C:25](=O)[CH2:26]Br)=[CH:23][CH:22]=1.C(O)(=O)C>O1CCOCC1>[CH3:18][O:17][C:13]1[CH:14]=[CH:15][CH:16]=[C:3]([O:2][CH3:1])[C:4]=1[CH2:5][NH:6][C:7]([NH:8][C:9]1[S:10][CH:26]=[C:25]([C:24]2[CH:29]=[CH:30][C:21]([C:20]([F:19])([F:31])[F:32])=[CH:22][CH:23]=2)[N:11]=1)=[NH:12]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 3219792-Bromo-4'-(trifluoromethyl)acetophenoneHCID 178491371HCID 178491371、化合物

生成物 1

HCID 178491357HCID 178491357、化合物収率 52.9%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

Preparation took place analogously to Example 3 by reaction of 140 mg (0.52 mmol) N-[[(2,6-dimethoxybenzyl)amino](imino)methyl]thiourea with 140 mg (0.52 mmol) 4-(trifluoromethyl)phenacyl bromide. The educts were suspended in 3 ml dioxane, were added to 0.3 ml acetic acid and were heated for 40 minutes in the microwave (radiation 300 Watt). The mixture was subsequently concentrated and the crude product obtained was purified by chromatography on silica gel (dichloromethane/methanol 1-4%). Stirring of the yellow foam obtained with methyl tert.-butyl ether yielded 120 mg of a white amorphous solid.

後処理

  1. customPreparation
  2. temperaturewere heated for 40 minutes in the microwave (radiation 300 Watt)
  3. concentrationThe mixture was subsequently concentrated
  4. customthe crude product obtained
  5. customwas purified by chromatography on silica gel (dichloromethane/methanol 1-4%)
  6. customobtained with methyl tert.-butyl ether

出典と根拠

ORDレコード
ord-18bb78271e744dd0b06c3577ed06103e
出典データセット
uspto-grants-2013_04
特許番号
US08431604B2

関連ノート

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