1-Methylpiperazine → (E)-Methyl 11-(4-methylpiperazin-1-yl)dibenzo[b,f][1,4]oxazepine-8-carboxylate

HRID 1907778노트

반응식

HRID 1907778 반응식
Cl[C:2]1=[N:3][C:4]2[CH:16]=[C:15]([C:17]([O:19][CH3:20])=[O:18])[CH:14]=[CH:13][C:5]=2[O:6][C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][C:8]1=2.[CH3:21][N:22]1[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]1>C1(C)C=CC=CC=1>[CH3:21][N:22]1[CH2:27][CH2:26][N:25]([C:2]2=[N:3][C:4]3[CH:16]=[C:15]([C:17]([O:19][CH3:20])=[O:18])[CH:14]=[CH:13][C:5]=3[O:6][C:7]3[CH:12]=[CH:11][CH:10]=[CH:9][C:8]2=3)[CH2:24][CH2:23]1

참가 물질

4

반응물 2

HCID 531671-MethylpiperazineHCID 58875660(E)-Methyl 11-chlorodibenzo[b,f][1,4]oxazepine-8-carboxylate

생성물 1

HCID 59737449(E)-Methyl 11-(4-methylpiperazin-1-yl)dibenzo[b,f][1,4]oxazepine-8-carboxylate수율 66.5%

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
110 °C

실험 절차

Compound 549 (1.06 g, 3.68 mmol) and 1-methylpiperazine (0.818 mL, 7.37 mmol) were dissolved in toluene (40 mL) and stirred at 110° C. for 16 h. The toluene was removed on the rotary evaporator. The crude product was dissolved in ethyl acetate and washed with water. The organic layer was separated and dried with Na2SO4, filtered and concentrated via rotary evaporation. The residue was purified via Isco employing a 0 to 50% methanol:ethyl acetate solvent gradient to afford compound 550 (0.86 g, 66%) as a white solid.

후처리

  1. customThe toluene was removed on the rotary evaporator
  2. dissolutionThe crude product was dissolved in ethyl acetate
  3. washwashed with water
  4. customThe organic layer was separated
  5. dry with materialdried with Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated via rotary evaporation
  8. customThe residue was purified via Isco

출처 및 근거

ORD 기록
ord-8e24ad2d7b6f41a68296d7665452ade8
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08598168B2

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