Methyl iodide → 1163123-55-4

HRID 598520

반응식

HRID 598520 반응식
[F:1][C:2]1[C:3]([F:12])=[CH:4][C:5]2[S:9][C:8]([SH:10])=[N:7][C:6]=2[CH:11]=1.[C:13](=O)([O-])[O-].[K+].[K+].IC>CN(C)C=O.O>[F:1][C:2]1[C:3]([F:12])=[CH:4][C:5]2[S:9][C:8]([S:10][CH3:13])=[N:7][C:6]=2[CH:11]=1

참가 물질

6

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 178505403HCID 178505403, 화합물

생성물 1

HCID 448201041163123-55-4수율 91.7%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

반응 조건

온도
0 °C

실험 절차

A suspension (0° C.) of 300 mg (1.476 mmol) 5,6-difluoro-benzothiazole-2-thiol and 306 mg (2.214 mmol) potassium carbonate in 6 mL N,N-dimethylformamide under nitrogen, were added 110.5 μL (1.77 mmol) iodomethane. The mixture was stirred at 0° C. for 1 h. The mixture was diluted with water (30 mL) and extracted with ethyl acetate. The combined extracts were washed with water and brine, dried over Na2SO4, filtered and concentrated in vacuo to provide 294 mg (91.7%) of the title compound as a solid. MS(m/e): 218.3 (M+H+).

후처리

  1. extractionextracted with ethyl acetate
  2. washThe combined extracts were washed with water and brine
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-42fff5004a39426cbcdd2fc6075afefb
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07897627B2

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