Sodium Iodide → HCID 67811489, 화합물

HRID 923656노트

반응식

HRID 923656 반응식
Cl[CH2:2][C:3]([N:5]1[CH2:10][CH2:9][N:8]([C:11]([O:13][CH2:14][CH3:15])=[O:12])[CH2:7][CH2:6]1)=[O:4].[I-:16].[Na+]>CC(C)=O>[I:16][CH2:2][C:3]([N:5]1[CH2:10][CH2:9][N:8]([C:11]([O:13][CH2:14][CH3:15])=[O:12])[CH2:7][CH2:6]1)=[O:4]

참가 물질

4

반응물 2

HCID 5238Sodium IodideHCID 2063649HCID 2063649, 화합물

생성물 1

HCID 67811489HCID 67811489, 화합물수율 75.3%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of ethyl 4-(2-chloroacetyl)piperazine-1-carboxylate (2.36 g, 10.06 mmol) and sodium iodide (3 g, 20.11 mmol) in acetone (45 mL) was stirred at room temperature for 24 h to give a suspension containing white solids. The solids were removed by filtration, and the filtrate was concentrated under reduced pressure. The residue was extracted with CH2Cl2 and H2O. The organic layer then dried over MgSO4, filtered and concentrated to give ethyl 4-(2-iodoacetyl)piperazine-1-carboxylate (2.47 g, 75% yield). C9H151N2O3; brown oil; IR vmax (neat) 2981, 2927, 2864, 1697, 1642, 1464, 1434, 1385, 1286, 1232, 1133, 1073, 1030, 989, 767 cm−1; 1H NMR (400 MHz, CDCl3) δ 4.14 (2H, q, J=7.0 Hz), 3.75 (2H, s), 3.58 (4H, m), 3.43 (4H, m), 1.26 (3H, t, J=7.0 Hz); 13C NMR (100 MHz, CDCl3) δ 166.6, 155.1, 61.8, 47.0, 43.1 (2×), 42.0 (2×), 14.7; ESI-HRMS calcd for C9H161N2O3: 327.0206. found: m/z 327.0215 [M+H]+.

후처리

  1. customto give a suspension
  2. additioncontaining white solids
  3. customThe solids were removed by filtration
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. extractionThe residue was extracted with CH2Cl2 and H2O
  6. dry with materialThe organic layer then dried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-593a04203fe04e6b9bb369ad8e7051e7
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09278982B2

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