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

HRID 1271277노트

반응식

HRID 1271277 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-b7c34754af254a2e9272709fe1e0424b
출처 데이터셋
uspto-grants-2007_04
특허 번호
US07205302B2

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