HCID 178477641, 화합물 → HCID 178477637, 화합물

HRID 1671649노트

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HRID 1671649 반응식
[CH2:1]([S:3]([C:6]1[CH:33]=[CH:32][C:9]([O:10][C:11]2[C:12]([CH:26]([OH:31])[CH2:27][CH2:28][CH2:29]O)=[CH:13][C:14]3[N:18]=[C:17]([C:19]4[CH:24]=[CH:23][CH:22]=[CH:21][N:20]=4)[NH:16][C:15]=3[CH:25]=2)=[CH:8][CH:7]=1)(=[O:5])=[O:4])[CH3:2]>C(Cl)(Cl)Cl>[O:31]1[CH2:29][CH2:28][CH2:27][CH:26]1[C:12]1[C:11]([O:10][C:9]2[CH:32]=[CH:33][C:6]([S:3]([CH2:1][CH3:2])(=[O:5])=[O:4])=[CH:7][CH:8]=2)=[CH:25][C:15]2[NH:16][C:17]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][N:20]=3)=[N:18][C:14]=2[CH:13]=1

참가 물질

3

반응물 1

HCID 178477641HCID 178477641, 화합물

생성물 1

HCID 178477637HCID 178477637, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

P-toluenesulfonic acid monohydrate (20 mg) was added to a chloroform (4 ml) solution of 1-(6-(4-(ethylsulfonyl)phenoxy)-2-pyridin-2-yl-1H-benzimidazol-5-yl)butane-1,4-diol (81 mg) obtained in (step 1), and the reaction liquid was stirred overnight with heating under reflux. The solvent was evaporated away under reduced pressure, and the reaction mixture was purified through reversed-phase middle-pressure liquid chromatography (ODS-AS-360-CC (by YMC), mobile phase: water/acetonitrile/0.1% trifluoroacetic acid), and the resulting fraction was diluted with ethyl acetate, washed with aqueous saturated sodium bicarbonate and saturated saline water in that order, and dried with anhydrous sodium sulfate. The solvent was evaporated away under reduced pressure to obtain the entitled compound as a white solid.

후처리

  1. customobtained in (step 1)
  2. customthe reaction liquid
  3. temperaturewith heating
  4. temperatureunder reflux
  5. customThe solvent was evaporated away under reduced pressure
  6. customthe reaction mixture was purified through reversed-phase middle-pressure liquid chromatography (ODS-AS-360-CC (by YMC), mobile phase: water/acetonitrile/0.1% trifluoroacetic acid)
  7. additionthe resulting fraction was diluted with ethyl acetate
  8. washwashed with aqueous saturated sodium bicarbonate and saturated saline water in that order
  9. dry with materialdried with anhydrous sodium sulfate
  10. customThe solvent was evaporated away under reduced pressure

출처 및 근거

ORD 기록
ord-5e033d5453d3454c83ae6a87d8b736ad
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07994331B2

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