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Sodium Hydroxide → HCID 66621883, 화합물

HRID 415993
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HRID 415993 반응식
C[O:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([C:11]2[CH:16]=[C:15]([Cl:17])[C:14]([CH2:18][C@@H:19]3[CH2:23][CH2:22][N:21]([CH:24]4[CH2:29][CH2:28][O:27][CH2:26][CH2:25]4)[C:20]3=[O:30])=[C:13]([Cl:31])[CH:12]=2)=[CH:7][CH:6]=1)=[O:4].[OH-].[Na+]>CO>[Cl:17][C:15]1[CH:16]=[C:11]([C:8]2[CH:7]=[CH:6][C:5]([C:3]([OH:4])=[O:2])=[CH:10][CH:9]=2)[CH:12]=[C:13]([Cl:31])[C:14]=1[CH2:18][C@@H:19]1[CH2:23][CH2:22][N:21]([CH:24]2[CH2:25][CH2:26][O:27][CH2:28][CH2:29]2)[C:20]1=[O:30]
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반응물 2

HCID 14798Sodium HydroxideHCID 666221203',5'-dichloro-4'-[(R)-2-oxo-1-(tetrahydro-pyran-4-yl)-pyrrolidin-3-ylmethyl]-biphenyl-4-carboxylic acid methyl ester

생성물 1

HCID 66621883HCID 66621883, 화합물수율 100.6%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Treat a solution of 3′,5′-dichloro-4′-[(R)-2-oxo-1-(tetrahydro-pyran-4-yl)-pyrrolidin-3-ylmethyl]-biphenyl-4-carboxylic acid methyl ester (2.56 g, 5.5 mmol) in methanol (25 mL) with 5N aqueous sodium hydroxide (5.5 mL). Heat the reaction to 60° C. and stir for 1 hr. Cool to room temperature, quench with 1N hydrochloric acid and extract the aqueous with ethyl acetate. Wash the organic layer with brine, dry over magnesium sulfate, and filter. Remove the solvent under vacuum to afford 2.48 g (100%) of desired product: MS (m/z): 448 (M+).

후처리

  1. temperatureHeat
  2. customthe reaction to 60° C.
  3. customquench with 1N hydrochloric acid
  4. extractionextract the aqueous with ethyl acetate
  5. washWash the organic layer with brine
  6. dry with materialdry over magnesium sulfate
  7. filtrationfilter
  8. customRemove the solvent under vacuum

출처 및 근거

ORD 기록
ord-b3ccfb779cdf4b29ae2b19be9cfa34d2
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08088776B2

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