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Hydrochloric Acid → HCID 178516220, 화합물

HRID 491827
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HRID 491827 반응식
[O:1]=[C:2]1[CH2:6][CH2:5][CH2:4][N:3]1[C@H:7]1[CH2:12][CH2:11][C@H:10]([C:13]([O:15]C)=[O:14])[CH2:9][CH2:8]1.[OH-].[Na+].Cl.[Cl-].[Na+]>CO>[O:1]=[C:2]1[CH2:6][CH2:5][CH2:4][N:3]1[C@H:7]1[CH2:12][CH2:11][C@H:10]([C:13]([OH:15])=[O:14])[CH2:9][CH2:8]1
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참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 5234Sodium ChlorideHCID 14798Sodium HydroxideHCID 178501171HCID 178501171, 화합물

생성물 1

HCID 178516220HCID 178516220, 화합물수율 97.9%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Methyl trans-4-(2-oxo-pyrrolidin-1-yl)cyclohexanecarboxylate (39.15 g) obtained in Reference Example 113(3) dissolved in methanol (400 ml), and thereto is added 2 N aqueous sodium hydroxide solution (60 ml) and the mixture is stirred at room temperature for 3 hours. The reaction solution is adjusted to pH 1-2 by pouring 10% hydrochloric acid under ice-cooling, saturated with sodium chloride, and then extracted with chloroform. The organic layer is dried over sodium sulfate, and then evaporated to remove the solvent under reduced pressure. The resulting residue is suspended in a small amount of ethyl acetate, and diisopropyl ether is poured thereto, and the resulting crystals are collected by filtration. The crystals are washed with diisopropyl ether several times and dried to give the title compound (35.94 g).

후처리

  1. extractionextracted with chloroform
  2. dry with materialThe organic layer is dried over sodium sulfate
  3. customevaporated
  4. customto remove the solvent under reduced pressure
  5. additionis poured
  6. filtrationthe resulting crystals are collected by filtration
  7. washThe crystals are washed with diisopropyl ether several times
  8. customdried

출처 및 근거

ORD 기록
ord-1bd5f03802ac41e1856205f8bb565b72
출처 데이터셋
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07531537B2

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