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Hydrochloric Acid → {3'-[4-(1-Ethyl-1H-pyrazol-4-ylmethyl)-piperazin-1-yl]-3,4,5,6-tetrahydro-2H-[1,2']bipyridinyl-4-yl}-methanol hydrochloride

HRID 604316
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HRID 604316 반응식
[N:1]1([C:7]2[C:8]([N:13]3[CH2:18][CH2:17][CH:16]([CH2:19][OH:20])[CH2:15][CH2:14]3)=[N:9][CH:10]=[CH:11][CH:12]=2)[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.[CH2:21]([N:23]1[CH:27]=[C:26]([CH:28]=O)[CH:25]=[N:24]1)[CH3:22].C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].[OH-].[Na+].[ClH:46]>ClCCCl.C(#N)C.C(Cl)Cl>[ClH:46].[CH2:21]([N:23]1[CH:27]=[C:26]([CH2:28][N:4]2[CH2:3][CH2:2][N:1]([C:7]3[C:8]([N:13]4[CH2:14][CH2:15][CH:16]([CH2:19][OH:20])[CH2:17][CH2:18]4)=[N:9][CH:10]=[CH:11][CH:12]=3)[CH2:6][CH2:5]2)[CH:25]=[N:24]1)[CH3:22]
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참가 물질

9

반응물 5

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 27589001-Ethyl-1H-pyrazole-4-carboxaldehydeHCID 5049666Sodium triacetoxyborohydrideHCID 59438214(3'-piperazin-1-yl-3,4,5,6-tetrahydro-2H-[1,2']bipyridinyl-4-yl)-methanol

생성물 1

HCID 67038358
{3'-[4-(1-Ethyl-1H-pyrazol-4-ylmethyl)-piperazin-1-yl]-3,4,5,6-tetrahydro-2H-[1,2']bipyridinyl-4-yl}-methanol hydrochloride
수율 97.3%

시약·촉매·용매 3

HCID 111,2-Dichloroethane용매HCID 6342Acetonitrile용매HCID 6344Dichloromethane용매

실험 절차

To a solution of (3′-piperazin-1-yl-3,4,5,6-tetrahydro-2H-[1,2′]bipyridinyl-4-yl)-methanol (0.145 g, 0.524 mmol, 1 eq) and 1-ethyl-1H-pyrazole-4-carbaldehyde (97.69 mg, 0.787 mmol, 1.5 eq) in 1,2-dichloroethane (10 mL) add sodium triacetoxyborohydride (166.79 mg, 0.787 mmol, 1.5 eq) in one portion as a solid. Stir the mixture at room temperature under nitrogen for 20 hr. Add 2 M aqueous sodium hydroxide solution (20 ml) and DCM (20 ml). Separate using a phase separator and extract the aqueous layer with DCM (10 ml). Concentrate the combined organic extracts and purify by high pH reverse phase HPLC. Dissolve this material (120 mg, 0.31 mmol) in the minimum quantity of 50% aqueous acetonitrile. Add 2 M aqueous hydrogen chloride (155 μL, 0.31 mmol) and lyophilize to give the title compound (127 mg, 58%). MS (m/z): 385.2 (M+1).

후처리

  1. customSeparate
  2. extractionextract the aqueous layer with DCM (10 ml)
  3. concentrationConcentrate the combined organic extracts
  4. custompurify by high pH reverse phase HPLC

출처 및 근거

ORD 기록
ord-e96090f8338c4161a4926bd870298725
출처 데이터셋
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07910588B2

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