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Lithium Hydroxide → HCID 59416009, 화합물

HRID 2061864
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HRID 2061864 반응식
[CH3:1][O:2][CH2:3][CH:4]([N:8]1[C:17]2[C:12](=[CH:13][C:14]([I:18])=[CH:15][CH:16]=2)[C:11](=[O:19])[C:10]([C:20]([O:22]CC)=[O:21])=[CH:9]1)[CH2:5][O:6][CH3:7].[OH-].[Li+]>O1CCCC1.O>[CH3:1][O:2][CH2:3][CH:4]([N:8]1[C:17]2[C:12](=[CH:13][C:14]([I:18])=[CH:15][CH:16]=2)[C:11](=[O:19])[C:10]([C:20]([OH:22])=[O:21])=[CH:9]1)[CH2:5][O:6][CH3:7]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 59415956HCID 59415956, 화합물2회

생성물 1

HCID 59416009HCID 59416009, 화합물수율 75%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

Ethyl 1-(1,3-dimethoxypropan-2-yl)-6-iodo-4-oxo-1,4-dihydroquinoline-3-carboxylate (Intermediate 22, 270 mg, 0.60 mmol) was dissolved in tetrahydrofuran (20 mL) and water (5 mL). Lithium hydroxide (56 mg, 2.42 mmol) was added and the mixture was stirred for 10 min at room temperature. The reaction mixture was then refluxed at 80° C. for 1 h. The reaction mixture was concentrated under reduced pressure and water (10 mL) was added. The pH was adjusted to 2 with hydrochloric acid (2N) and the solid that precipitated was collected by filtration and dried to afford 185 mg (75%) of 1-(1,3-dimethoxypropan -2-yl)-6-iodo-4-oxo-1,4-dihydroquinoline-3-carboxylic acid.

후처리

  1. temperatureThe reaction mixture was then refluxed at 80° C. for 1 h
  2. concentrationThe reaction mixture was concentrated under reduced pressure and water (10 mL)
  3. additionwas added
  4. customthe solid that precipitated
  5. filtrationwas collected by filtration
  6. customdried

출처 및 근거

ORD 기록
ord-a86ba0cba9ad4aeeae4361c3d7e875b3
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08283361B2

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