Methylamine → 8-(N-Methyl)aminomethyl-10-methoxymethyl-10H-pyrazino[2,3-b][1,4]benzothiazine

HRID 1059426노트

반응식

HRID 1059426 반응식
Cl[CH2:2][C:3]1[CH:4]=[CH:5][C:6]2[S:11][C:10]3[N:12]=[CH:13][CH:14]=[N:15][C:9]=3[N:8]([CH2:16][O:17][CH3:18])[C:7]=2[CH:19]=1.[CH3:20][NH2:21]>CO>[CH3:20][NH:21][CH2:2][C:3]1[CH:4]=[CH:5][C:6]2[S:11][C:10]3[N:12]=[CH:13][CH:14]=[N:15][C:9]=3[N:8]([CH2:16][O:17][CH3:18])[C:7]=2[CH:19]=1

참가 물질

4

반응물 2

HCID 6329MethylamineHCID 1133536310-methoxymethyl-8-chloromethyl-10H-pyrazino[2,3-b][1,4]benzothiazine

생성물 1

HCID 186703078-(N-Methyl)aminomethyl-10-methoxymethyl-10H-pyrazino[2,3-b][1,4]benzothiazine

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

8-Chloromethyl-10-methoxymethyl-10H-pyrazino[2,3-b][1,4]benzothiazine was stirred in a solution of methylamine in methanol at room temperature over day and night. Then the reaction mixture was distilled under reduced pressure and the residue was distributed into sodium hydroxide and ethyl acetate. The organic layer was extracted and dried over anhydrous sodium sulfate. After distilling off the solvent under reduced pressure, the obtained residue was purified by silica gel column chromatography (eluted with dichloromethane/methanol) to thereby give the title compound as a yellow oily substance.

후처리

  1. distillationThen the reaction mixture was distilled under reduced pressure
  2. extractionThe organic layer was extracted
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationAfter distilling off the solvent under reduced pressure
  5. customthe obtained residue was purified by silica gel column chromatography (eluted with dichloromethane/methanol)

출처 및 근거

ORD 기록
ord-1d5af62ee1cb45208655f8c0f8690b15
출처 데이터셋
uspto-grants-2003_02
특허 번호
US06518423B1

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