Hydrochloric Acid → (S)-3-[(R)-1-(3-methoxyphenyl)ethylamino]pyrrolidine dihydrochloride

HRID 1811643

反応式

HRID 1811643 の反応式
C([N:8]1[CH2:12][CH2:11][C@H:10]([NH:13][C@@H:14]([C:16]2[CH:21]=[CH:20][CH:19]=[C:18]([O:22][CH3:23])[CH:17]=2)[CH3:15])[CH2:9]1)C1C=CC=CC=1.[ClH:24]>CO.O1CCOCC1.[OH-].[Pd+2].[OH-]>[ClH:24].[ClH:24].[CH3:23][O:22][C:18]1[CH:17]=[C:16]([C@H:14]([NH:13][C@H:10]2[CH2:11][CH2:12][NH:8][CH2:9]2)[CH3:15])[CH:21]=[CH:20][CH:19]=1

参加物

6

反応物 2

HCID 313Hydrochloric AcidHCID 58973545(S)-(1-benzylpyrrolidin-3-yl)-[(R)-1-(3-methoxyphenyl)ethyl]amine

生成物 1

HCID 67408353(S)-3-[(R)-1-(3-methoxyphenyl)ethylamino]pyrrolidine dihydrochloride

試薬・触媒・溶媒 3

HCID 9942167Palladium hydroxide触媒HCID 887Methanol溶媒HCID 312751,4-Dioxane溶媒

実験手順

To a solution of 3.67 g of (S)-(1-benzylpyrrolidin-3-yl)-[(R)-1-(3-methoxyphenyl)ethyl]amine dissolved in 100 ml of methanol were added 830 mg of palladium hydroxide and 8.85 ml of a solution of 4M hydrochloric acid in dioxane, and the mixture was shaked under hydrogen atmosphere at 3 atm at room temperature for 3 days. Palladium hydroxide was removed, and the solvent was evaporated. To the residue was added methanol, and the resulting precipitates were collected by filtration, washed with methanol and dried to obtain 1.14 g of (S)-3-[(R)-1-(3-methoxyphenyl)ethylamino]pyrrolidine dihydrochloride (the following Reference example Table, Reference example 1.001).

後処理

  1. customPalladium hydroxide was removed
  2. customthe solvent was evaporated
  3. additionTo the residue was added methanol
  4. customthe resulting precipitates
  5. filtrationwere collected by filtration
  6. washwashed with methanol
  7. customdried

出典と根拠

ORDレコード
ord-6e9fee769062453794fd522f467877a0
出典データセット
uspto-grants-2013_01
特許番号
US08362274B2

関連ノート

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