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Hydrochloric Acid → HCID 70175216, 화합물

HRID 2186347
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HRID 2186347 반응식
[OH-].[Na+].[CH3:3][O:4][C:5]1[CH:6]=[C:7]2[C:12](=[CH:13][CH:14]=1)[N:11]=[CH:10][CH:9]=[C:8]2[CH2:15][CH2:16][CH2:17][C@@H:18]1[CH2:23][CH2:22][N:21]([CH2:24][CH2:25][S:26][C:27]2[S:28][CH:29]=[CH:30][CH:31]=2)[CH2:20][C@@H:19]1[C:32]([O:34]C)=[O:33].[ClH:36]>CO.O.ClCCl.CO>[ClH:36].[ClH:36].[CH3:3][O:4][C:5]1[CH:6]=[C:7]2[C:12](=[CH:13][CH:14]=1)[N:11]=[CH:10][CH:9]=[C:8]2[CH2:15][CH2:16][CH2:17][C@@H:18]1[CH2:23][CH2:22][N:21]([CH2:24][CH2:25][S:26][C:27]2[S:28][CH:29]=[CH:30][CH:31]=2)[CH2:20][C@@H:19]1[C:32]([OH:34])=[O:33]
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참가 물질

7

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 86758151HCID 86758151, 화합물

생성물 1

HCID 70175216HCID 70175216, 화합물

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매
HCID 21226129
Dichloromethane methanol
용매

반응 조건

온도
60 °C

실험 절차

0.5 cm3 of 5N aqueous sodium hydroxide was added to a stirred solution of 0.34 g of methyl (3R,4R)-4-[3-(6-methoxyquinolin-4-yl)propyl]-1-[2-(thien-2-ylthio)ethyl]piperidine-3-carboxylate in 3 cm3 of methanol and then the mixture was heated at a temperature in the region of 60° C. for 20 hours. After evaporating the solvents under reduced pressure (5 kPa) at a temperature in the region of 40° C., the residue obtained was taken up in 5 cm3 of water and then acidified by addition of 1 cm3 of 35% hydrochloric acid. The mixture was again evaporated under reduced pressure under the same conditions as above; the residue obtained was taken up in 5 cm3 of a dichloromethane/methanol (90/10 by volume) mixture. The insoluble material was filtered off and then the solvent was evaporated under reduced pressure (5 kPa) at a temperature in the region of 40° C. 0.35 g of (3R,4R)-4-[3-(6-methoxyquinolin-4-yl)propyl]-1-[2-(thien-2-ylthio)ethyl]piperidine-3-carboxylic acid dihydrochloride was obtained in the form of a solid with a beige color which melts with softening in the region of 150° C.

후처리

  1. customAfter evaporating the solvents under reduced pressure (5 kPa) at a temperature in the region of 40° C.
  2. customthe residue obtained
  3. customThe mixture was again evaporated under reduced pressure under the same conditions as above
  4. customthe residue obtained
  5. filtrationThe insoluble material was filtered off
  6. customthe solvent was evaporated under reduced pressure (5 kPa) at a temperature in the region of 40° C

출처 및 근거

ORD 기록
ord-4cb9062afb35435aa589966af6b91900
출처 데이터셋
uspto-grants-2002_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06403610B1

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