Hydrochloric Acid → (R)-N-(2-((10,11-Dihydro-5H-dibenzo[a,d]cyclohepten-5-ylidene)methoxy)ethyl)-3-piperidinecarboxylic acid hydrochloride

HRID 2226753노트

반응식

HRID 2226753 반응식
C([O:3][C:4]([C@@H:6]1[CH2:11][CH2:10][CH2:9][N:8]([CH2:12][CH2:13][O:14][CH:15]=[C:16]2[C:22]3[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=3[CH2:20][CH2:19][C:18]3[CH:27]=[CH:28][CH:29]=[CH:30][C:17]2=3)[CH2:7]1)=[O:5])C.[OH-].[Na+].O.[ClH:34]>C(O)C.ClCCl>[ClH:34].[CH:27]1[C:18]2[CH2:19][CH2:20][C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=3[C:16](=[CH:15][O:14][CH2:13][CH2:12][N:8]3[CH2:9][CH2:10][CH2:11][C@@H:6]([C:4]([OH:5])=[O:3])[CH2:7]3)[C:17]=2[CH:30]=[CH:29][CH:28]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 14798Sodium HydroxideHCID 11761301(R)-N-(2-((10,11-dihydro-5H-dibenzo [a, d]cyclohepten-5-ylidene)methoxy)ethyl)-3-piperidinecarboxylic acid ethyl ester

생성물 1

HCID 45264517(R)-N-(2-((10,11-Dihydro-5H-dibenzo[a,d]cyclohepten-5-ylidene)methoxy)ethyl)-3-piperidinecarboxylic acid hydrochloride

시약·촉매·용매 2

HCID 702Ethanol용매HCID 6344Dichloromethane용매

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온도
50 °C

실험 절차

The above ester (2.0 g, 4.9 mmol) was dissolved in ethanol (20 ml) and a 4 N sodium hydroxide solution (4.9 ml) was added. The mixture was stirred at 50° C. for 2 h. Water (10 ml) was added and ethanol was evaporated in vacuo to give an aqueous residue. A 4 M aqueous hydrochloric acid solution (6.2 ml) was added followed by dichloromethane (50 ml). The phases were separated and the aqueous phase was extracted with dichloromethane (50 ml). The combined organic phases were washed with water (10 ml) and then dried over magnesium sulphate. The solvent was evaporated in vacuo and the residue dried in vacuo to give 1.71 g of the title compound as a solid.

후처리

  1. customethanol was evaporated in vacuo
  2. customto give an aqueous residue
  3. customThe phases were separated
  4. extractionthe aqueous phase was extracted with dichloromethane (50 ml)
  5. washThe combined organic phases were washed with water (10 ml)
  6. dry with materialdried over magnesium sulphate
  7. customThe solvent was evaporated in vacuo
  8. customthe residue dried in vacuo

출처 및 근거

ORD 기록
ord-e012b1090b164fa18eb7f4f26ba53a68
출처 데이터셋
uspto-grants-1994_09
특허 번호
US05348965

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