Acetic Acid → HCID 178491357, 화합물

HRID 447919

반응식

HRID 447919 반응식
[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]

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 3219792-Bromo-4'-(trifluoromethyl)acetophenoneHCID 178491371HCID 178491371, 화합물

생성물 1

HCID 178491357HCID 178491357, 화합물수율 52.9%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9072fbad3f304c2c9ddca3e721445ed0
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08481576B2

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