HCID 68513291、化合物 → HCID 58852308、化合物

HRID 1716578ノート

反応式

HRID 1716578 の反応式
C(OC([N:8]1[CH2:13][CH2:12][CH:11]([N:14]2[C:18]3[CH:19]=[CH:20][C:21]([CH3:23])=[CH:22][C:17]=3[N:16]=[C:15]2[C:24](=[O:26])[CH3:25])[CH2:10][CH2:9]1)=O)(C)(C)C>FC(F)(F)C(O)=O.C(Cl)Cl>[CH3:23][C:21]1[CH:20]=[CH:19][C:18]2[N:14]([CH:11]3[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]3)[C:15]([C:24](=[O:26])[CH3:25])=[N:16][C:17]=2[CH:22]=1

参加物

4

反応物 1

HCID 68513291HCID 68513291、化合物

生成物 1

HCID 58852308HCID 58852308、化合物収率 100%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 6422Trifluoroacetic acid溶媒

実験手順

4-(2-acetyl-5-methyl-benzoimidazol-1-yl)-piperidine-1-carboxylic acid tert-butyl ester (107 mg, 0.30 mmol) was dissolved in a mixture of trifluoroacetic acid (2 mL) and CH2Cl2 (2 mL) at rt and stirred for 1 hour. The mixture was concentrated under reduced pressure and the residue was partitioned between dilute aqueous K2CO3 solution (20 mL) and CH2Cl2 (20 mL). The organic layer was separated, and the aqueous layer was extracted with CH2Cl2 (2×15 mL). The combined organic layers were dried over anhydrous Na2SO4 and concentrated under reduced pressure to give 1-(5-methyl-1-piperidin-4-yl-1H-benzoimidazol-2-yl)-ethanone as an oil (77 mg, 0.30 mmol, 100%) that was used without further purification or characterization.

後処理

  1. concentrationThe mixture was concentrated under reduced pressure
  2. customthe residue was partitioned between dilute aqueous K2CO3 solution (20 mL) and CH2Cl2 (20 mL)
  3. customThe organic layer was separated
  4. extractionthe aqueous layer was extracted with CH2Cl2 (2×15 mL)
  5. dry with materialThe combined organic layers were dried over anhydrous Na2SO4
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-db18570768d94ff4b8c81fc86864ddb6
出典データセット
uspto-grants-2010_09
特許番号
US07803816B2

反応ノート

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