Benzenesulfonyl chloride → HCID 59859943、化合物

HRID 2174950ノート

反応式

HRID 2174950 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 59859943HCID 59859943、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

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)+.

後処理

  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)

出典と根拠

ORDレコード
ord-7db1d4af3a2049ada70bec6008e9cbe7
出典データセット
uspto-grants-2015_06
特許番号
US09062046B2

反応ノート

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