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Lithium hydroxide, monohydrate → HCID 71087846, 화합물

HRID 927510
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HRID 927510 반응식
C[O:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([CH:11]2[CH2:15][CH2:14][O:13][CH2:12]2)=[C:7]([C:16]2[CH:21]=[CH:20][CH:19]=[C:18]([Cl:22])[CH:17]=2)[N:6]=1)=[O:4].O.[OH-].[Li+]>CO.C(OCC)(=O)C>[Cl:22][C:18]1[CH:17]=[C:16]([C:7]2[N:6]=[C:5]([C:3]([OH:4])=[O:2])[CH:10]=[CH:9][C:8]=2[CH:11]2[CH2:15][CH2:14][O:13][CH2:12]2)[CH:21]=[CH:20][CH:19]=1
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참가 물질

4

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 71087516HCID 71087516, 화합물

생성물 1

HCID 71087846HCID 71087846, 화합물수율 81%

시약·촉매·용매 1

HCID 21584119Ethylacetate methanol용매

실험 절차

A mixture of 6-(3-chlorophenyl)-5-(tetrahydrofuran-3-yl)-pyridine-2-carboxylic acid methyl ester (0.15 g, 0.5 mmol) and lithium hydroxide monohydrate (CAN 1310-66-3, 88 mg, 2.1 mmol) in THF/H2O 1/1 (20 mL)) was stirred at room temperature for 1 h. After removal of the organic solvent under reduced pressure, the aqueous phase was washed with ethyl acetate (10 mL) and acidified with 1 N HCl to pH=3. The resulting solution was extracted with ethyl acetate (2×20 mL). The combined organic layer was concentrated under reduced pressure to provide the title compound (0.12 g, 81%) as black oil which was used in the next step without further purification; MS (EI): m/e=304.1 [M+H]+.

후처리

  1. customAfter removal of the organic solvent under reduced pressure
  2. washthe aqueous phase was washed with ethyl acetate (10 mL)
  3. extractionThe resulting solution was extracted with ethyl acetate (2×20 mL)
  4. concentrationThe combined organic layer was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-9e5a780ffece43b2a6e6a6c47d7dd003
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09290451B2

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