ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Dichloromethane → 2-(6-(4-Methanesulfonyl-phenoxy)-2-pyridin-2-yl-3H-benzimidazol-5-yl)-pyrrolidine-1-carboxamide

HRID 13284
ノート
印刷プレビュー

反応式

HRID 13284 の反応式
CN(C1C=CC=CN=1)C.C[Si]([N:14]=[C:15]=[O:16])(C)C.C(Cl)Cl.[CH3:20][S:21]([C:24]1[CH:50]=[CH:49][C:27]([O:28][C:29]2[C:43]([CH:44]3[CH2:48][CH2:47][CH2:46][NH:45]3)=[CH:42][C:32]3[NH:33][C:34]([C:36]4[CH:41]=[CH:40][CH:39]=[CH:38][N:37]=4)=[N:35][C:31]=3[CH:30]=2)=[CH:26][CH:25]=1)(=[O:23])=[O:22]>O>[CH3:20][S:21]([C:24]1[CH:25]=[CH:26][C:27]([O:28][C:29]2[C:43]([CH:44]3[CH2:48][CH2:47][CH2:46][N:45]3[C:15]([NH2:14])=[O:16])=[CH:42][C:32]3[NH:33][C:34]([C:36]4[CH:41]=[CH:40][CH:39]=[CH:38][N:37]=4)=[N:35][C:31]=3[CH:30]=2)=[CH:49][CH:50]=1)(=[O:22])=[O:23]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6344DichloromethaneHCID 218852-DimethylaminopyridineHCID 70696Trimethylsilyl isocyanateHCID 231451755-(4-methanesulfonyl-phenoxy)-2-pyridin-2-yl-6-pyrrolidin-2-yl-1H-benzimidazole

生成物 1

HCID 114089432-(6-(4-Methanesulfonyl-phenoxy)-2-pyridin-2-yl-3H-benzimidazol-5-yl)-pyrrolidine-1-carboxamide

試薬・触媒・溶媒 1

HCID 962
Water
溶媒

実験手順

5 mg of dimethylaminopyridine and 0.029 ml of trimethylsilyl isocyanate were added to a methylene chloride (1 ml) solution of 17.1 mg of 5-(4-methanesulfonyl-phenoxy)-2-pyridin-2-yl-6-pyrrolidin-2-yl-1H-benzimidazole obtained in Example 162 (step 7), and the reaction liquid was stirred overnight at room temperature. Water was added to the reaction liquid, and extracted with ethyl acetate, and then washed with saturated saline. After dried and concentrated, the resulting residue 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 in 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. customthe reaction liquid
  2. extractionextracted with ethyl acetate
  3. washwashed with saturated saline
  4. customAfter dried
  5. concentrationconcentrated
  6. customthe resulting residue 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 in 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-7819c548dc1b40ea81bc958cbf8fcd01
出典データセット
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07728025B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート