Sodium Bicarbonate → (+/-)-4-[1-(5,6-Diphenylpyrazin-2-yl)pyrrolidin-2-yl]-1-butanol

HRID 1271277ノート

反応式

HRID 1271277 の反応式
[C:1]1([C:7]2[N:8]=[CH:9][C:10]([N:19]3[CH2:23][CH2:22][CH2:21][CH:20]3[CH2:24][CH2:25][CH2:26][CH2:27][O:28]C3CCCCO3)=[N:11][C:12]=2[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.O.C1(C)C=CC(S(O)(=O)=O)=CC=1.C(=O)([O-])O.[Na+]>CO>[C:1]1([C:7]2[N:8]=[CH:9][C:10]([N:19]3[CH2:23][CH2:22][CH2:21][CH:20]3[CH2:24][CH2:25][CH2:26][CH2:27][OH:28])=[N:11][C:12]=2[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

5

反応物 3

HCID 516892Sodium BicarbonateHCID 521998p-Toluenesulfonic acid monohydrateHCID 22931951(+/-)-1-[1-(5,6-Diphenylpyrazin-2-yl)pyrrolidin-2-yl]-4-(2-tetrahydropyranyloxy)butane

生成物 1

HCID 18452667(+/-)-4-[1-(5,6-Diphenylpyrazin-2-yl)pyrrolidin-2-yl]-1-butanol収率 107.8%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 1.25 g of (±)-1-[1-(5,6-diphenylpyrazin-2-yl)pyrrolidin-2-yl]-4-(2-tetrahydropyranyloxy)butane in 13 ml of methanol, 0.52 g of p-toluenesulfonic acid monohydrate was added, followed by stirring at room temperature for 3 hours. The reaction solution was alkalified by adding an aqueous saturated sodium hydrogen carbonate solution, and then extracted with ethyl acetate. The extract was dried over anhydrous magnesium sulfate and the solvent was evaporated under reduced pressure to obtain 1.10 g of the desired compound as a pale yellow oily substance.

後処理

  1. extractionextracted with ethyl acetate
  2. dry with materialThe extract was dried over anhydrous magnesium sulfate
  3. customthe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-b7c34754af254a2e9272709fe1e0424b
出典データセット
uspto-grants-2007_04
特許番号
US07205302B2

反応ノート

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