HCID 68513291, 화합물 → HCID 58852308, 화합물

HRID 1716578노트

반응식

HRID 1716578 반응식
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

참가 물질

4

반응물 1

HCID 68513291HCID 68513291, 화합물

생성물 1

HCID 58852308HCID 58852308, 화합물수율 100%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 6422Trifluoroacetic acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-db18570768d94ff4b8c81fc86864ddb6
출처 데이터셋
uspto-grants-2010_09
특허 번호
US07803816B2

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