Potassium Hydroxide → HCID 66811476, 화합물

HRID 1099203노트

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HRID 1099203 반응식
[C:1]([N:4]1[CH2:8][CH2:7][CH:6]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[C:5]1(C(OCC)=O)[C:15]([O:17]CC)=[O:16])(=[O:3])[CH3:2].[OH-].[K+]>C(O)C>[C:1]([N:4]1[CH2:8][CH2:7][CH:6]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[C@H:5]1[C:15]([OH:17])=[O:16])(=[O:3])[CH3:2]

참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 11056701HCID 11056701, 화합물

생성물 1

HCID 66811476HCID 66811476, 화합물수율 95%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
0 °C

실험 절차

To a solution of diethyl 1-acetyl-3-phenylpyrrolidine-2,2-dicarboxylate (110.6 g, 331 mmol) in ethanol (500 ml) was added potassium hydroxide (55.7 g, 993 mmol). The reaction was allowed to stir at reflux for 8 h and was then concentrated. The residue was dissolved in water and extracted with EtOAc. The aqueous layer was cooled to 0° C., carefully acidified to pH 2-3 using conc HCl, and exhaustively extracted with EtOAc. The combined organics were dried over sodium sulfate, filtered, and concentrated in vacuo to yield 1-acetyl-3-phenylproline as a solid (95%).

후처리

  1. temperatureat reflux for 8 h
  2. concentrationwas then concentrated
  3. dissolutionThe residue was dissolved in water
  4. extractionextracted with EtOAc
  5. extractionexhaustively extracted with EtOAc
  6. dry with materialThe combined organics were dried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-5e4bc14cce7b455b89fdc1e26b4266e1
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08143405B2

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