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Dimethylformamide → HCID 69597599, 화합물

HRID 1796809
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인쇄 미리보기

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HRID 1796809 반응식
CN(C)C=O.[CH3:6][NH:7][C:8]([N:10]1[CH2:15][CH2:14][N:13]([S:16]([C:19]2[CH:24]=[CH:23][C:22]([OH:25])=[CH:21][CH:20]=2)(=[O:18])=[O:17])[CH:12]([C:26]23[O:33][CH2:32][C:29]([CH3:34])([CH2:30][O:31]2)[CH2:28][O:27]3)[CH:11]1[CH3:35])=[O:9].C(=O)([O-])[O-].[Cs+].[Cs+].Br[CH2:43][C:44]1[CH:49]=[C:48]([F:50])[CH:47]=[CH:46][C:45]=1[CH3:51]>C(OCC)(=O)C>[CH3:6][NH:7][C:8]([N:10]1[CH2:15][CH2:14][N:13]([S:16]([C:19]2[CH:24]=[CH:23][C:22]([O:25][CH2:43][C:44]3[CH:49]=[C:48]([F:50])[CH:47]=[CH:46][C:45]=3[CH3:51])=[CH:21][CH:20]=2)(=[O:18])=[O:17])[CH:12]([C:26]23[O:33][CH2:32][C:29]([CH3:34])([CH2:28][O:27]2)[CH2:30][O:31]3)[CH:11]1[CH3:35])=[O:9]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 10796Cesium carbonateHCID 27746055-Fluoro-2-methylbenzyl bromideHCID 69597610HCID 69597610, 화합물

생성물 1

HCID 69597599HCID 69597599, 화합물수율 95.6%

시약·촉매·용매 1

HCID 8857Ethyl Acetate
용매

반응 조건

온도
45 °C

실험 절차

To a N,N-dimethylformamide (1.5 ml) solution of 4-(4-Hydroxy-benzenesulfonyl)-2-methyl-3-(4-methyl-2,6,7-trioxa-bicyclo[2.2.2]oct-1-yl)-piperazine-1-carboxylic acid methylamide (compound of formula XLV, 0.31 g, 0.7 mmol) was added cesium carbonate (0.45 g) and 2-bromomethyl-4-fluoro-1-methyl-benzene (0.214 g, 1.05 mmol). The reaction mixture was stirred at about 45° C. for about 16 hours and then was allowed to cool and was diluted with ethyl acetate and washed with water. The organic layer was dried with sodium sulfate and concentrated in vacuo to give 0.377 g of a compound of formula XLIV.

후처리

  1. temperatureto cool
  2. washwashed with water
  3. dry with materialThe organic layer was dried with sodium sulfate
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-fa88237a17f14c83b18183d5449495c2
출처 데이터셋
uspto-grants-2006_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07030242B2

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