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Dichloromethane → HCID 23564544, 화합물

HRID 1059421
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HRID 1059421 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[NH:7][CH2:8][C:9]([C:11]1[CH:12]=[CH:13][C:14]2[S:19][C:18]3[N:20]=[CH:21][CH:22]=[N:23][C:17]=3[N:16](COC)[C:15]=2[CH:27]=1)=O.S(Cl)(Cl)=O.ClCCl>C(Cl)(Cl)(Cl)Cl>[N:7]1[CH:8]=[C:9]([C:11]2[CH:12]=[CH:13][C:14]3[S:19][C:18]4[N:20]=[CH:21][CH:22]=[N:23][C:17]=4[NH:16][C:15]=3[CH:27]=2)[N:1]2[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=12
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6344DichloromethaneHCID 24386Thionyl ChlorideHCID 23565187[N-(2-Pyridyl)aminometyl](10-methoxymethyl-10H-pyrazino[2,3-b][1,4]benzothiazin-8-yl)ketone

생성물 1

HCID 23564544HCID 23564544, 화합물수율 61.6%

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

실험 절차

10 ml of a solution of 200 mg of [N-(2-pyridyl)aminometyl](10-methoxymethyl-10H-pyrazino[2,3-b][1,4]benzothiazin-8-yl)ketone in carbon tetrachloride was stirred at room temperature and 240 mg of thionyl chloride was dropped thereinto. The reaction mixture was distributed into dichloromethane and an aqueous solution of sodium bicarbonate and the organic layer was separated. To the organic layer were added methanol and tetrahydrofuran to give a homogeneous solution. After adding silica gel and distilling off the solvent under reduced pressure, the residue was purified by silica gel column chromatography (eluted with dichloromethane/methanol) to thereby give 103 mg of the title compound as yellow crystals.

후처리

  1. customan aqueous solution of sodium bicarbonate and the organic layer was separated
  2. additionTo the organic layer were added methanol and tetrahydrofuran
  3. customto give a homogeneous solution
  4. additionAfter adding silica gel
  5. distillationdistilling off the solvent under reduced pressure
  6. customthe residue was purified by silica gel column chromatography (eluted with dichloromethane/methanol)

출처 및 근거

ORD 기록
ord-ce1339966b1f4c70899cfbbe10757b5f
출처 데이터셋
uspto-grants-2003_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06518423B1

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