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Lithium Hydroxide → HCID 22933861, 화합물

HRID 1269801
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HRID 1269801 반응식
[NH:1]1[C:9]2[C:4](=[CH:5][C:6]([O:10][CH:11]3[CH2:16][CH2:15][CH:14]([C:17]([O:19]CC)=[O:18])[CH2:13][CH2:12]3)=[CH:7][CH:8]=2)[CH:3]=[N:2]1.[OH-].[Li+]>CO.O1CCCC1>[NH:1]1[C:9]2[C:4](=[CH:5][C:6]([O:10][CH:11]3[CH2:12][CH2:13][CH:14]([C:17]([OH:19])=[O:18])[CH2:15][CH2:16]3)=[CH:7][CH:8]=2)[CH:3]=[N:2]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 22934049HCID 22934049, 화합물

생성물 1

HCID 22933861HCID 22933861, 화합물수율 58%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

The ethyl 4-(1H-indazol-5-yloxy)cyclo-hexanecarboxylate (728.4 mg, 2.53 mmol) obtained in Example 367 was dissolved in a mixture of methanol (2.5 ml) and tetrahydrofuran (2.5 ml), and a 2M-aqueous lithium hydroxide solution (2.53 ml, 5.05 mmol) was added dropwise thereto. After 2 hours, the reaction mixture was concentrated under reduced pressure and the resulting residue was dissolved in water (5 ml). The resulting aqueous solution was adjusted to pH 4 with a 0.5M-aqueous potassium hydrogensulfate solution. The crystals formed were filtered under reduced pressure and then dried to obtain 4-(1H-indazol-5-yloxy)cyclohexanecarboxylic acid (381 mg, 58%).

후처리

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. dissolutionthe resulting residue was dissolved in water (5 ml)
  3. customThe crystals formed
  4. filtrationwere filtered under reduced pressure
  5. customdried

출처 및 근거

ORD 기록
ord-b630d4a84dc642d2b34cee7f48e5d07f
출처 데이터셋
uspto-grants-2007_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07199147B2

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