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

HRID 1907778ノート

反応式

HRID 1907778 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
110 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8e24ad2d7b6f41a68296d7665452ade8
出典データセット
uspto-grants-2013_12
特許番号
US08598168B2

反応ノート

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