Hydrochloric Acid → HCID 66785056、化合物

HRID 1096598ノート

反応式

HRID 1096598 の反応式
[CH3:1][O:2][CH2:3][CH2:4][CH2:5][N:6]1[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[N:8]=[C:7]1[C@@H:15]1[CH2:20][CH2:19][CH2:18][N:17](C(OC(C)(C)C)=O)[CH2:16]1.Cl>CCO>[CH3:1][O:2][CH2:3][CH2:4][CH2:5][N:6]1[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[N:8]=[C:7]1[C@@H:15]1[CH2:20][CH2:19][CH2:18][NH:17][CH2:16]1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 66786343(R)-tert-butyl 3-(1-(3-methoxypropyl)-1H-benzo[d]imidazol-2-yl)piperidine-1-carboxylate

生成物 1

HCID 66785056HCID 66785056、化合物収率 99%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

(R)-tert-Butyl 3-(1-(3-methoxypropyl)-1H-benzo[d]imidazol-2-yl)piperidine-1-carboxylate (4.82 mmol; 1.8 g) was added to a 100 mL round-bottomed flask equipped with a reflux condenser and stirring under nitrogen. EtOH (15 mL) and HCl (8 M in H2O; 4 mL) were then added and the solution was heated to reflux for 10 min. Analysis of the reaction mixture by LC/MS indicated that the reaction was complete. The solvent was then removed in-vacuo. The resultant oil was then extracted with EtOAc and a 10% aqueous K2CO3 solution. The organic layer was collected and dried with Na2SO4, and was then filtered. The filtrate was concentrated and dried in-vacuo affording (R)-1-(3-methoxypropyl)-2-(piperidin-3-yl)-1H-benzo[d]imidazole (7D) as a brown oil (4.76 mmol, 1.3 g, 99% yield). ESI-MS: m/z 274.4 (M+H)+.

後処理

  1. customequipped with a reflux condenser
  2. temperaturethe solution was heated
  3. temperatureto reflux for 10 min
  4. customThe solvent was then removed in-vacuo
  5. extractionThe resultant oil was then extracted with EtOAc
  6. customThe organic layer was collected
  7. dry with materialdried with Na2SO4
  8. filtrationwas then filtered
  9. concentrationThe filtrate was concentrated
  10. customdried in-vacuo

出典と根拠

ORDレコード
ord-85b5fcc0fc0040f2a73f811adea3dee8
出典データセット
uspto-grants-2012_03
特許番号
US08138168B1

反応ノート

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