Benzenesulfonyl chloride → HCID 59859943, 화합물

HRID 2174950노트

반응식

HRID 2174950 반응식
[Br:1][C:2]1[CH:3]=[C:4]([NH2:10])[C:5]([O:8][CH3:9])=[N:6][CH:7]=1.[C:11]1([S:17](Cl)(=[O:19])=[O:18])[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1>N1C=CC=CC=1>[Br:1][C:2]1[CH:3]=[C:4]([NH:10][S:17]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)(=[O:19])=[O:18])[C:5]([O:8][CH3:9])=[N:6][CH:7]=1

참가 물질

4

반응물 2

HCID 7369Benzenesulfonyl chlorideHCID 447548695-Bromo-2-methoxypyridin-3-amine

생성물 1

HCID 59859943HCID 59859943, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

5-bromo-2-methoxypyridin-3-amine (1.231 mmol) was dissolved in pyridine (3 ml) at 0° C. Benzene sulfonyl chloride (1.847 mmol) was added drop wise and the reaction mixture was stirred at RT for 2 h. The reaction mixture was evaporated to dryness and the residue was dissolved in ethyl acetate (100 mL). The ethyl acetate layer was washed with water, separated and dried over sodium sulfate. The organic layer was evaporated to dryness. The crude material obtained was purified by (silica column, EtOAc/Hexane as eluent) to obtain the title compound. 1HNMR (300 MHz, DMSO-d6): δ 10.16 (s, 1H), 8.05 (d, J=2.4 Hz, 1H), 7.77 (m, 2H), 7.68 (d, J=2.4 Hz, 1H), 7.64 (m, 1H), 7.55 (m, 1H), 3.61 (s, 3H); MS (m/z): 343 (M)+.

후처리

  1. customThe reaction mixture was evaporated to dryness
  2. dissolutionthe residue was dissolved in ethyl acetate (100 mL)
  3. washThe ethyl acetate layer was washed with water
  4. customseparated
  5. dry with materialdried over sodium sulfate
  6. customThe organic layer was evaporated to dryness
  7. customThe crude material obtained
  8. customwas purified by (silica column, EtOAc/Hexane as eluent)

출처 및 근거

ORD 기록
ord-7db1d4af3a2049ada70bec6008e9cbe7
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09062046B2

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