Pyridine → 8-Chloromethyl-10H-pyrazino[2,3-b][1,4]benzothiazine

HRID 1059273노트

반응식

HRID 1059273 반응식
[N:1]1[C:10]2[NH:9][C:8]3[CH:11]=[C:12]([CH2:15]O)[CH:13]=[CH:14][C:7]=3[S:6][C:5]=2[N:4]=[CH:3][CH:2]=1.N1C=CC=CC=1.CS([Cl:27])(=O)=O.C(Cl)Cl.C(=O)([O-])O.[Na+]>CN(C)C=O>[Cl:27][CH2:15][C:12]1[CH:13]=[CH:14][C:7]2[S:6][C:5]3[N:4]=[CH:3][CH:2]=[N:1][C:10]=3[NH:9][C:8]=2[CH:11]=1

참가 물질

6

반응물 4

HCID 1049PyridineHCID 31297Methanesulfonyl chlorideHCID 1094429210H-Pyrazino[2,3-b][1,4]benzothiazine-8-methanolHCID 23716255Sodium bicarbonate methylene chloride

생성물 1

HCID 117470388-Chloromethyl-10H-pyrazino[2,3-b][1,4]benzothiazine

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Into a solution of 7 g of 10H-pyrazino[2,3-b][1,4]benzothiazine-8-methanol and 6.1 ml of pyridine in N,N-dimethylformamide (50 ml) was added dropwise 5.9 ml of methanesulfonyl chloride at 0° C. After stirring at room temperature for 1 hour, the reaction mixture was poured into a pre-cooled aqueous solution of methylene chloride/sodium hydrogencarbonate, extracted with ethyl acetate, washed with water and dried over anhydrous sodium sulfate. After distilling off the solvent under reduced pressure, the crystals thus precipitated were diluted with a small amount of ethyl acetate, taken up by filtration and washed with diethyl ether. Thus 4.7 g of the title compound was obtained as a yellow powder.

후처리

  1. extractionextracted with ethyl acetate
  2. washwashed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationAfter distilling off the solvent under reduced pressure
  5. customthe crystals thus precipitated
  6. additionwere diluted with a small amount of ethyl acetate
  7. filtrationtaken up by filtration
  8. washwashed with diethyl ether

출처 및 근거

ORD 기록
ord-acf4eca3cbe3444dbf31cd03ab5bdd33
출처 데이터셋
uspto-grants-2003_02
특허 번호
US06518423B1

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