Ethanol hydrochloride → ethyl (S)-3-(2-amino-1,2,3,4-tetrahydronaphthalen-7-yl)propionate

HRID 369363ノート

反応式

HRID 369363 の反応式
C(OC([NH:8][C@H:9]1[CH2:18][CH2:17][C:16]2[C:11](=[CH:12][C:13]([CH2:19][CH2:20][C:21]([O:23][CH2:24][CH3:25])=[O:22])=[CH:14][CH:15]=2)[CH2:10]1)=O)(C)(C)C.C(O)C.Cl>C(O)C>[NH2:8][C@H:9]1[CH2:18][CH2:17][C:16]2[C:11](=[CH:12][C:13]([CH2:19][CH2:20][C:21]([O:23][CH2:24][CH3:25])=[O:22])=[CH:14][CH:15]=2)[CH2:10]1

参加物

4

反応物 2

HCID 21887872Ethanol hydrochlorideHCID 57250977ethyl (S)-3-[2-(tert-butoxycarbonylamino)-1,2,3,4-tetrahydronaphthalen-7-yl]propionate

生成物 1

HCID 53933206ethyl (S)-3-(2-amino-1,2,3,4-tetrahydronaphthalen-7-yl)propionate収率 100.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Ethyl (S)-3-[2-(tert-butoxycarbonylamino)-1,2,3,4-tetrahydronaphthalen-7-yl]propionate (1.47 g) was dissolved in ethanol (21 ml), and 3 M hydrogen chloride ethanol solution (4 ml) was added to the solution at room temperature with stirring. After reaction for 20 hours, the reaction mixture was concentrated in vacuo. A saturated aqueous sodium bicarbonate solution (50 ml) and dichloromethane (10 ml) were added to the residue, and the resulting mixture was stirred for an hour at room temperature. Water was added to the reaction mixture, and the resulting mixture was extracted with dichloromethane. The extract was washed with water and dried over anhydrous magnesium sulfate. Removal of the solvent in vacuo gave ethyl (S)-3-(2-amino-1,2,3,4-tetrahydronaphthalen-7-yl)propionate (1.05 g) as an oil.

後処理

  1. customAfter reaction for 20 hours
  2. concentrationthe reaction mixture was concentrated in vacuo
  3. additionA saturated aqueous sodium bicarbonate solution (50 ml) and dichloromethane (10 ml) were added to the residue
  4. stirringthe resulting mixture was stirred for an hour at room temperature
  5. additionWater was added to the reaction mixture
  6. extractionthe resulting mixture was extracted with dichloromethane
  7. washThe extract was washed with water
  8. dry with materialdried over anhydrous magnesium sulfate
  9. customRemoval of the solvent in vacuo

出典と根拠

ORDレコード
ord-2604fc55ba65488f8d320432692ab8c0
出典データセット
uspto-grants-2000_10
特許番号
US06136852

反応ノート

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