Ethanol → HCID 9947152, 화합물

HRID 1795585노트

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HRID 1795585 반응식
[CH2:1](N(C1C(C)=CC2C(C)CCC(C)(C)C=2C=1)C1C=CC(C(OCC)=O)=CC=1)C.C([N:31]([C:43]1[C:52]([CH3:53])=[CH:51][C:50]2[C:49]([CH3:55])([CH3:54])[CH2:48][CH:47]=[C:46]([CH3:56])[C:45]=2[CH:44]=1)[C:32]1[CH:42]=[CH:41][C:35]([C:36]([O:38][CH2:39][CH3:40])=[O:37])=[CH:34][CH:33]=1)C.C(O)C.[OH-].[K+]>O>[CH2:56]([C:46]1[C:45]2[CH:44]=[C:43]([NH:31][C:32]3[CH:33]=[CH:34][C:35]([C:36]([O:38][CH2:39][CH3:40])=[O:37])=[CH:41][CH:42]=3)[C:52]([CH3:53])=[CH:51][C:50]=2[C:49]([CH3:54])([CH3:55])[CH2:48][CH:47]=1)[CH3:1]

참가 물질

6

반응물 4

HCID 702EthanolHCID 14797Potassium HydroxideHCID 10270958HCID 10270958, 화합물HCID 22218330Ethyl 4-[ethyl(3,5,8,8-tetramethyl-5,6-dihydronaphthalen-2-yl)amino]benzoate

생성물 1

HCID 9947152HCID 9947152, 화합물수율 92%

시약·촉매·용매 1

HCID 962Water용매

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온도
60 °C

실험 절차

General Procedure E To a solution of ethyl 4-[ethyl(3,5,8,8-tetramethyl-5,6-dihydronaphthalen-2-yl)amino]benzoate, (Compound 19, 0.17 g, 0.45 mmol) and 5 mL of absolute ethyl alcohol was added aqueous 5 M KOH (2 mL). The resulting solution was heated in an 60° C. bath for 24 h. The solution was cooled to room temperature, diluted with water and washed once with 2:1 hexane:ethyl acetate solution, and the layers were separated. The aqueous layer was acidified with HCl 2 N to pH=0-1 and the product extracted three times with ethyl acetate. The combined organic extracts were washed with brine, dried over MgSO4, and filtered. The solvent was removed to give 0.042 g (92%) of the title compound as an off-white solid.

후처리

  1. temperatureThe solution was cooled to room temperature
  2. washwashed once with 2:1 hexane
  3. customethyl acetate solution, and the layers were separated
  4. extractionthe product extracted three times with ethyl acetate
  5. washThe combined organic extracts were washed with brine
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. customThe solvent was removed

출처 및 근거

ORD 기록
ord-094fad334df14da2ab8d8e6eaa0796ff
출처 데이터셋
uspto-grants-2006_04
특허 번호
US07026487B2

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