Cesium carbonate → HCID 89650133, 화합물

HRID 1479030

반응식

HRID 1479030 반응식
[CH2:1]([O:3][C:4](=[O:12])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1F)[CH3:2].[NH:13]1[CH:17]=[CH:16][N:15]=[C:14]1[CH2:18][N:19]([CH3:21])[CH3:20].C(=O)([O-])[O-].[Cs+].[Cs+]>CS(C)=O.CC(=O)OCC>[CH2:1]([O:3][C:4](=[O:12])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[N:13]1[CH:17]=[CH:16][N:15]=[C:14]1[CH2:18][N:19]([CH3:21])[CH3:20])[CH3:2]

참가 물질

6

반응물 3

HCID 10796Cesium carbonateHCID 67953Benzoic acid, 2-fluoro-, ethyl esterHCID 11457689((1H-imidazol-2-yl)methyl)dimethylamine

생성물 1

HCID 89650133HCID 89650133, 화합물수율 18%

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 8857Ethyl Acetate용매

반응 조건

온도
120 °C

실험 절차

A mixture of 2-fluoro-benzoic acid ethyl ester (200 mg; 1.19 mmol; 10 eq.), (1H-imidazol-2-ylmethyl)-dimethyl-amine (149 mg; 1.19 mmol; 1 eq.) and cesium carbonate (775 mg; 2.38 mmol; 2 eq.) in DMSO (3 mL) was stirred at 120° C. for 16 hours. The mixture was diluted with EA, washed with water (3×), dried over magnesium sulfate and concentrated in vacuo to afford the title compound (58 mg, 18%) as a white solid. HPLC (max plot) 95.7%; Rt 1.80 min.

후처리

  1. washwashed with water (3×)
  2. dry with materialdried over magnesium sulfate
  3. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-d63f11815a5f4e159cf2a7763df8b5aa
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09403835B2

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