HCID 178477641、化合物 → HCID 178477637、化合物

HRID 1671649ノート

反応式

HRID 1671649 の反応式
[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

参加物

3

反応物 1

HCID 178477641HCID 178477641、化合物

生成物 1

HCID 178477637HCID 178477637、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5e033d5453d3454c83ae6a87d8b736ad
出典データセット
uspto-grants-2011_08
特許番号
US07994331B2

反応ノート

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