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1-Piperazinecarboxylic acid, ethyl ester → Ethyl 4-{[2-(3-chlorophenyl)-2H-tetrazol-5-yl]methyl}piperazine-1-carboxylate

HRID 639798
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HRID 639798 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([N:8]2[N:12]=[N:11][C:10]([CH:13]=O)=[N:9]2)[CH:5]=[CH:6][CH:7]=1.[CH2:15]([O:17][C:18]([N:20]1[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]1)=[O:19])[CH3:16].C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(OCC)(=O)C>ClCCCl>[Cl:1][C:2]1[CH:3]=[C:4]([N:8]2[N:12]=[N:11][C:10]([CH2:13][N:23]3[CH2:22][CH2:21][N:20]([C:18]([O:17][CH2:15][CH3:16])=[O:19])[CH2:25][CH2:24]3)=[N:9]2)[CH:5]=[CH:6][CH:7]=1
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참가 물질

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반응물 4

HCID 84311-Piperazinecarboxylic acid, ethyl esterHCID 8857Ethyl AcetateHCID 5049666Sodium triacetoxyborohydrideHCID 594242182-(3-chlorophenyl)-2H-tetrazole-5-carbaldehyde

생성물 1

HCID 11537602Ethyl 4-{[2-(3-chlorophenyl)-2H-tetrazol-5-yl]methyl}piperazine-1-carboxylate수율 46.4%

시약·촉매·용매 1

HCID 11
1,2-Dichloroethane
용매

실험 절차

2-(3-Chloro-phenyl)-2H-tetrazole-5-carbaldehyde (22.3 mg, 0.107 mmol) was dissolved in 1,2-dichloroethane under argon and ethyl-1-piperazine carboxylate (16.4 uL, 0.112 mmol) was added followed by sodium triacetoxy borohydride (31.8 mg, 0.150 mmol). The reaction was allowed to stir overnight. Ethyl acetate was added and the solution was washed with sodium bicarbonate (sat.), brine, dried over sodium sulfate, filtered and concentrated. The crude product was purified by column chromatography using 45% EtOAc/Hexanes and 100% EtOAc to yield the title compound as a white solid (17.4 mg, 46%). 1H NMR (CDCl3) δ (ppm): 8.190 (s, 1H); 8.070 (m, 1H); 7.469 (m, 2H); 4.139 (q, 2H); 3.983 (s, 2H); 3.541 (m, 4H); 2.604 (m, 4H); 1.263 (t, 3H).

후처리

  1. washthe solution was washed with sodium bicarbonate (sat.), brine
  2. dry with materialdried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe crude product was purified by column chromatography

출처 및 근거

ORD 기록
ord-05bdfaf63fed4ee09655467473eb9d18
출처 데이터셋
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07691892B2

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