Lithium hydroxide, monohydrate → HCID 68089228, 화합물

HRID 1615688노트

반응식

HRID 1615688 반응식
[CH3:1][N:2]1[C:14]2[C:5](=[C:6]3[C:11](=[CH:12][CH:13]=2)[N:10]=[CH:9][CH:8]=[CH:7]3)[N:4]=[C:3]1[CH:15]([CH3:21])[CH2:16][C:17]([O:19]C)=[O:18].O.[OH-].[Li+]>C(#N)C.O>[CH3:1][N:2]1[C:14]2[C:5](=[C:6]3[C:11](=[CH:12][CH:13]=2)[N:10]=[CH:9][CH:8]=[CH:7]3)[N:4]=[C:3]1[CH:15]([CH3:21])[CH2:16][C:17]([OH:19])=[O:18]

참가 물질

5

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 68089342HCID 68089342, 화합물

생성물 1

HCID 68089228HCID 68089228, 화합물수율 90.5%

시약·촉매·용매 2

HCID 962Water용매HCID 6342Acetonitrile용매

실험 절차

To a solution of methyl 3-(3-methyl-3H-imidazo[4,5-f]quinolin-2-yl)butanoate (560 mg, 1.97 mmol) in acetonitrile (20 mL) and water (8 mL) was added lithium hydroxide hydrate (249 mg, 5.94 mmol). The mixture was stirred at room temperature overnight. The mixture was concentrated to about 8 mL. The pH of the solution was adjusted to ˜4 with 1N HCl aqueous solution. The mixture was concentrated to dryness and to the residue was added 50 mL of DCM/MeOH v/v 10:1. The precipitate was removed by filtration and the filtrate was concentrated to dryness to give the product as a yellow solid (480 mg, 90% yield). ESI MS: m/z 270.1 [M+H]+.

후처리

  1. concentrationThe mixture was concentrated to about 8 mL
  2. concentrationThe mixture was concentrated to dryness and to the residue
  3. additionwas added 50 mL of DCM/MeOH v/v 10:1
  4. customThe precipitate was removed by filtration
  5. concentrationthe filtrate was concentrated to dryness

출처 및 근거

ORD 기록
ord-7910eb83d16d4cfdb1e35daf24aeb738
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08765760B2

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