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

HRID 2223871
ノート
印刷プレビュー

反応式

HRID 2223871 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-e31492b101284082967088fa9d8667a3
出典データセット
uspto-grants-2008_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07375115B2

反応ノート

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