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Diethyl Ether → 2-[1-[2-(Tert-butyldiphenylsiloxy)ethyl]cyclohexyl]ethylamine

HRID 2223871
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인쇄 미리보기

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HRID 2223871 반응식
[O:1]([CH2:19][CH2:20][C:21]1([CH2:27][CH2:28][N:29]2C(=O)C3=CC=CC=C3C2=O)[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22]1)[Si:2]([C:15]([CH3:18])([CH3:17])[CH3:16])([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.O.NN.C(OCC)C>C(O)C>[O:1]([CH2:19][CH2:20][C:21]1([CH2:27][CH2:28][NH2:29])[CH2:22][CH2:23][CH2:24][CH2:25][CH2:26]1)[Si:2]([C:15]([CH3:17])([CH3:18])[CH3:16])([C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 3283Diethyl EtherHCID 24654Hydrazine hydrate (1:1)HCID 59714868N-[2-[1-[2-(tert-Butyldiphenylsiloxy)ethyl]cyclohexyl]ethyl]-phthalimide

생성물 1

HCID 597149732-[1-[2-(Tert-butyldiphenylsiloxy)ethyl]cyclohexyl]ethylamine수율 104%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of N-[2-[1-[2(tert-butyldiphenylsiloxy)ethyl]cyclohexyl]-ethyl]phthalimide (1.52 g) dissolved in ethanol (30 mL) was added hydrazine monohydrate. The reaction solution was heated under reflux for 4 hours. To this was added diethyl ether and the insolbles were filtered off. The solvent was then distilled off under reduced pressure. To this was added chloroform, and the solution was made basic by addition of a 1N aqueous hydroxide solution. The solution was then extracted with chloroform. The organic layer was dried over anhydrous magnesium sulfate, filtered, and then, the solvent was distilled off under reduced pressure to give the title compound (1.20 g).

후처리

  1. temperatureThe reaction solution was heated
  2. temperatureunder reflux for 4 hours
  3. filtrationthe insolbles were filtered off
  4. distillationThe solvent was then distilled off under reduced pressure
  5. additionTo this was added chloroform
  6. additionthe solution was made basic by addition of a 1N aqueous hydroxide solution
  7. extractionThe solution was then extracted with chloroform
  8. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  9. filtrationfiltered
  10. distillationthe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-e31492b101284082967088fa9d8667a3
출처 데이터셋
uspto-grants-2008_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07375115B2

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