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Water → Ethyl 2-((diphenylmethylene)amino)-2-(pyrazin-2-yl)acetate

HRID 716025
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인쇄 미리보기

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HRID 716025 반응식
[C:1]1([C:7](=[N:14][CH2:15][C:16]([O:18][CH2:19][CH3:20])=[O:17])[C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Br[C:22]1[CH:27]=[N:26][CH:25]=[CH:24][N:23]=1.C(=O)([O-])[O-].[K+].[K+].O>[I-].C([N+](CCCC)(CCCC)CCCC)CCC.CN1CCCC1=O>[C:1]1([C:7](=[N:14][CH:15]([C:22]2[CH:27]=[N:26][CH:25]=[CH:24][N:23]=2)[C:16]([O:18][CH2:19][CH3:20])=[O:17])[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 319508Ethyl 2-(diphenylmethyleneamino)acetateHCID 6428002-Bromopyrazine

생성물 1

HCID 10246971Ethyl 2-((diphenylmethylene)amino)-2-(pyrazin-2-yl)acetate

시약·촉매·용매 2

HCID 67553Tetrabutylammonium Iodide
촉매
HCID 13387N-methyl-2-pyrrolidone용매

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온도
110 °C

실험 절차

A mixture of ethyl 2-((diphenylmethylene)amino)acetate (6.0 g, 22.47 mmol), 2-bromopyrazine (7.1 g, 44.90 mmol), potassium carbonate (9.30 g, 67.40 mmol) and tetrabutyl ammonium iodide (8.10 g, 22.40 mmol) in N-methyl-2-pyrrolidone (25 mL) was heated in a sealed tube at 110° C. for 16 hours. The mixture was poured into water (100 mL) and extracted with ethyl acetate (3×50 mL). The organic layers were washed with brine (25 mL) and dried over sodium sulfate. Removal of solvent under vacuum afforded crude product which was purified in Combi-Flash instrument using a gradient of methanol in chloroform. Yield: 4.90 g (63%). 1H NMR (300 MHz, DMSO-d6) δ: 1.16 (t, 3H), 4.07 (q, 2H), 5.26 (s, 1H), 7.18 (dd, 2H), 7.38-7.61 (m, 8H), 8.56 (d, 1H), 8.57 (d, 1H), 8.60 (s, 1H). MS (ES) MH+: 346.3 for C21H19N3O2.

후처리

  1. extractionextracted with ethyl acetate (3×50 mL)
  2. washThe organic layers were washed with brine (25 mL)
  3. dry with materialdried over sodium sulfate
  4. customRemoval of solvent under vacuum
  5. customafforded crude product which
  6. customwas purified in Combi-Flash instrument

출처 및 근거

ORD 기록
ord-094f83a8dfc0419ba98afa68f10fb329
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09187495B2

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