Pyridine → HCID 57675191, 화합물

HRID 490920노트

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HRID 490920 반응식
[CH3:1][S:2](Cl)(=[O:4])=[O:3].Cl.[CH2:7]([N:9]1[C:13]2[N:14]=[CH:15][C:16]([C:25]3[O:29][N:28]=[C:27]([CH2:30][CH:31]4[CH2:36][CH2:35][NH:34][CH2:33][CH2:32]4)[N:26]=3)=[C:17]([NH:18][CH:19]3[CH2:24][CH2:23][O:22][CH2:21][CH2:20]3)[C:12]=2[CH:11]=[N:10]1)[CH3:8].N1C=CC=CC=1>C(Cl)(Cl)Cl>[CH2:7]([N:9]1[C:13]2[N:14]=[CH:15][C:16]([C:25]3[O:29][N:28]=[C:27]([CH2:30][CH:31]4[CH2:36][CH2:35][N:34]([S:2]([CH3:1])(=[O:4])=[O:3])[CH2:33][CH2:32]4)[N:26]=3)=[C:17]([NH:18][CH:19]3[CH2:20][CH2:21][O:22][CH2:23][CH2:24]3)[C:12]=2[CH:11]=[N:10]1)[CH3:8]

참가 물질

5

반응물 3

HCID 1049PyridineHCID 31297Methanesulfonyl chlorideHCID 67529443HCID 67529443, 화합물

생성물 1

HCID 57675191HCID 57675191, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

Methanesulphonyl chloride (1.16 mmol) was added to a stirred solution of Intermediate 125 (0.033 mmol) and pyridine (0.5 ml) in chloroform (1 ml) at room temperature. After stirring at room temperature for 31 h, the reaction mixture was applied to a SPE cartridge (aminopropyl, 5 g) and the cartridge was eluted sequentially with chloroform, ethyl acetate and methanol. Fractions containing the desired product were evaporated in vacuo. The resulting residue was further purified on a SPE cartridge (silica, 1 g) eluting with a gradient of 30-100% ethyl acetate in petroleum ether to afford Example 176. LCMS showed MH+=490, TRET=2.97 min.

후처리

  1. washthe cartridge was eluted sequentially with chloroform, ethyl acetate and methanol
  2. additionFractions containing the desired product
  3. customwere evaporated in vacuo
  4. customThe resulting residue was further purified on a SPE cartridge (silica, 1 g)
  5. washeluting with a gradient of 30-100% ethyl acetate in petroleum ether
  6. customto afford Example 176
  7. customMH+=490, TRET=2.97 min.

출처 및 근거

ORD 기록
ord-25299d7b274e4f40b3f12ea1336439f2
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07528148B2

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