Ethyl Acetate → HCID 11740793, 화합물

HRID 2355002노트

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HRID 2355002 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].C[O:8][C:9](=O)[C:10]1[CH:15]=[CH:14][C:13]([O:16][C:17]2[CH:22]=[C:21]([C:23](=[O:30])[NH:24][C:25]3[S:26][CH:27]=[CH:28][N:29]=3)[CH:20]=[C:19]([O:31][CH:32]([CH3:34])[CH3:33])[CH:18]=2)=[N:12][CH:11]=1.C(=O)([O-])O.[Na+].C(OCC)(=O)C>O1CCCC1>[OH:8][CH2:9][C:10]1[CH:15]=[CH:14][C:13]([O:16][C:17]2[CH:22]=[C:21]([CH:20]=[C:19]([O:31][CH:32]([CH3:34])[CH3:33])[CH:18]=2)[C:23]([NH:24][C:25]2[S:26][CH:27]=[CH:28][N:29]=2)=[O:30])=[N:12][CH:11]=1

참가 물질

6

반응물 4

HCID 8857Ethyl AcetateHCID 516892Sodium BicarbonateHCID 10431879HCID 10431879, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 11740793HCID 11740793, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
0 °C

실험 절차

After adding 6.0 mg (0.16 mmol) of lithium aluminum hydride to a solution of 60.0 mg (0.15 mmol) of the 6-[3-isopropoxy-5-(thiazol-2-ylcarbamoyl)-phenoxy]-nicotinic acid methyl ester obtained in Production Example 65 in tetrahydrofuran (5.0 ml) while cooling on ice, the mixture was stirred at 0° C. for 1 hour. Saturated aqueous sodium hydrogencarbonate was added to the reaction mixture, extraction was performed with ethyl acetate, and the organic layer was dried and then concentrated under reduced pressure. The obtained residue was purified by silica gel chromatography (chloroform:methanol=30:1) to obtain the title compound as a white solid. The analysis data for the compound obtained in Production Example 66 are shown below.

후처리

  1. temperaturewhile cooling on ice
  2. customthe organic layer was dried
  3. concentrationconcentrated under reduced pressure
  4. customThe obtained residue was purified by silica gel chromatography (chloroform:methanol=30:1)

출처 및 근거

ORD 기록
ord-82a3651765ba4cd6a5ef4e5f26eec42d
출처 데이터셋
uspto-grants-2010_07
특허 번호
US07754743B2

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