Lithium hydroxide, monohydrate → HCID 71284456, 화합물

HRID 1481682노트

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HRID 1481682 반응식
[CH2:1]([C:3]1[CH:4]=[C:5]([C:21]([O:23]C)=[O:22])[C:6](=[O:20])[NH:7][C:8]=1[C:9]1[CH:10]=[C:11]2[C:16](=[CH:17][CH:18]=1)[N:15]([CH3:19])[CH2:14][CH2:13][CH2:12]2)[CH3:2].O[Li].O>C1COCC1.O>[CH2:1]([C:3]1[CH:4]=[C:5]([C:21]([OH:23])=[O:22])[C:6](=[O:20])[NH:7][C:8]=1[C:9]1[CH:10]=[C:11]2[C:16](=[CH:17][CH:18]=1)[N:15]([CH3:19])[CH2:14][CH2:13][CH2:12]2)[CH3:2]

참가 물질

5

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 71284791HCID 71284791, 화합물

생성물 1

HCID 71284456HCID 71284456, 화합물수율 63.9%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

반응 조건

온도
65 °C

실험 절차

To a suspension of methyl 5-ethyl-6-(1-methyl-1,2,3,4-tetrahydroquinolin-6-yl)-2-oxo-1,2-dihydropyridine-3-carboxylate (200 mg, 0.61 mmol) in THF (1 mL) and H2O (1 mL) was added LiOH—H2O (85 mg, 2.03 mmol, 3.3 eq) at room temperature. The reaction mixture was heated to 65° C. and stirred for 1 h. The reaction was monitored by LC-MS. Upon complete consumption of starting material, the reaction was quenched with 1N HCl (2 mL). The precipitate was collected by filtration then washed with Et2O to afford the title compound as a yellow solid (121 mg, 0.39 mmol, 14% over three steps).

후처리

  1. customUpon complete consumption of starting material
  2. customthe reaction was quenched with 1N HCl (2 mL)
  3. filtrationThe precipitate was collected by filtration
  4. washthen washed with Et2O

출처 및 근거

ORD 기록
ord-4f1afa430bdd4f8c9e28be484b172f05
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09409905B2

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