Potassium Hydroxide → HCID 18405668, 화합물

HRID 653964노트

반응식

HRID 653964 반응식
C([O:3][C:4](=[O:17])[CH2:5][CH2:6][CH:7]1[CH:14]2[CH2:15][CH:10]3[CH2:11][CH:12]([CH2:16][CH:8]1[CH2:9]3)[CH2:13]2)C.[OH-].[K+]>C(O)C>[CH:14]12[CH2:15][CH:10]3[CH2:11][CH:12]([CH2:16][CH:8]([CH2:9]3)[CH:7]1[CH2:6][CH2:5][C:4]([OH:17])=[O:3])[CH2:13]2

참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 53933676Ethyl tricyclo[3.3.1.13,7]decane-2-propanoate

생성물 1

HCID 18405668HCID 18405668, 화합물수율 99.1%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of tricyclo[3.3.1.1-3,7]decane-2-propanoic acid ethyl ester (0.011 mol, 2.68 g) in anhydrous ethanol (135 mL) was added potassium hydroxide (0.057 mol, 3.18 g) in several portions. The clear solution was heated at reflux for 1 h, cooled to ambient temperature, and concentrated. The yellow residue was partitioned with CH2Cl2 (100 mL) and water (50 mL), and the basic, aqueous phase extracted with CH2Cl2 (100 mL). The aqueous phase was re-acidified (pH 2) by the addition of 10% aqueous hydrochloric acid, and extracted with CH2Cl2 (3×50 mL). The combined organic extracts were dried (Na2SO4) and concentrated to provide tricyclo[3.3.1.1-3,7]decane-2-propanoic acid as a white solid (96%, 2.27 g). mp 115.5°-116° C.

후처리

  1. temperatureThe clear solution was heated
  2. temperatureat reflux for 1 h
  3. concentrationconcentrated
  4. customThe yellow residue was partitioned with CH2Cl2 (100 mL) and water (50 mL)
  5. extractionthe basic, aqueous phase extracted with CH2Cl2 (100 mL)
  6. additionby the addition of 10% aqueous hydrochloric acid
  7. extractionextracted with CH2Cl2 (3×50 mL)
  8. dry with materialThe combined organic extracts were dried (Na2SO4)
  9. concentrationconcentrated

출처 및 근거

ORD 기록
ord-828630fc34d44e92bbcf13244ec092bf
출처 데이터셋
uspto-grants-1992_07
특허 번호
US05128448

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